sulphuric acid handbook 1000265717 (1)

7/22/2019 Sulphuric Acid Handbook 1000265717 (1)

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SULPHURIC ACID

HANDBOOK


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Coal Age ^ Electric Railway Journal

Electrical \3iforld ^ Engineering News-Record

American Machinist^ The Contractor

Engineering S Mining Journal ^ Power

Metallurgical 6 Chemical Engineering

Electrical Merchandising

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SULPHUEIC ACIDHANDBOOK

'

-

BYTHOMAS J. SULLIVAN

WITH THB MINBBAL POINT SINC COlfPANT, A BUBBIDIARTOF THB MBW JBBBBT SINO COMPANY

First Edition

McGRAW-HILL BOOK COMPANY, Inc.239 WEST 39TH STREET. NEW YORK

LONDON: HILL PUBLISHING CO., Ltd.6 8 BOUVERIE ST., E. C.

1918


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4

Copyright, 1918, by theMcGraw-Hill Book Company, Inc.

THK MAPI.S3 PRKSS T O S K PA


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PREFACE

As sulphuric acid is one of the most important of chemicals,being an intermediate raw product, essential in most manu-acturing

processes, I think the appearance of this handbookdealing solely with sulphuric acid is well justified. In fact,m almost every industry some sulphuric acid is used and itbas been asserted that the consumption of sulphuric acid byany nation is a measure of its degree of industrial progress.This is certainly not strictlycorrect, but sulphuric acid formsthe starting point of,and is used in so many industries that thereis considerable element of truth in this statement. A fewexamples showing some of its important uses follows:(a) For decomposing salts with the production of nitric acid,

hydrochloric acid and sodium sulphate, thus indirectly in themanufacture of soda ash, soap, glass,bleaching powder, etc.(6) For the purification of most kinds of oil,including petro-eum

and tar oils.(c) For pickling (^.e.,cleaning) iron goods previous to tinning

Dr galvanizing.(d) As a drying agent in the production of organic dyes, on

vhich the textile industry depends to a large extent.{e) For rendering soluble mineral and animal phosphate

(superphosphate) for manures; thus agriculture absorbs largea.mounts, and consequently food stuffs are affected byBuctuations in the supply of this important chemical.(/) For the manufacture of nitric acid from Chile saltpetre:

nitric acid and sulphuric acid together are used in the nitrationof organic substances such as glycerine and cellulose formingnitro-glycerineand nitro-cellulose mainly used in the manu-acture

of explosives now in great demand. So, a copious

327320


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vi PREFACE

supplyof sulphuricacid is an absolute necessityor the explosiveindustry and any shortagein this supply would mean a shortagelof explosives. IWithout multiplyingexamplesof this nature, enough has beenisaid to indicate the complexityof modern industrial conditions,the interaction of one industry on the other, and finallythejoften obscure, but highlyimportant, part played by sulphuriqacid as an ultimate and absolutelyessential raw material oithese industries.

Owing to the enormous amount of literaturecontainingdaton sulphuricacid,it has become more and more difficultfor thbusy worker to gather from this mass of literature,he facwhich are of practicalnterest and use to him. Much valuablmaterial is of Uttle use because it is scattered through the litera-ure

and is therefore inaccessible.The publication of this handbook was undertaken as an

attempt to overcome this difficulty,t least in part. The scophas been limited almost entirelyto numerical data, inasmuclas such data cannot generallybe carried in mind, but must bareadily accessible for use. The specialinvestigatorwouldprobably always preferto go to the originalource for the information he wishes,so, to republishall matter of this kind wouldbe unnecessary and impracticable.The attempt has beenmade to select and tabulate only that which is of fairlygeneralinterest and utiUty and produce a convenient reference boojjof numerical data.

In collectingthe tables only those generallyadapted tcAmerican practicehave been selected. When specificravitis given in terms of the Baum6 degrees,the so-called AmericaStandard has been adhered to. Where a different Baumscale has been used in a table,the figureshave been recalculateto conform to the American Standard. Almost all of the tableof Bineau, Kolb, Otto, Winkler, Messel, Knietsch, PickerinLunge, Isler,Naef, etc.,have been omitted as they have Ionsince become obsolete as far as being of practicalalue for us


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PREFACE vii

n general American practioe. All molecular weights asirell as the factors for the calculation of analytical results haveeen calculated from the International Atomic Weights of 19171918). The molecular weights and other figures have beenarried out further beyond the decimal point than is necessaryor most calculations.Great care and pains have been taken. to secure accuracy

nd completeness of data. All figures have been calculatedeveral times, and it is hoped that the errors have been reduced0 the minimum. However, errors have undoubtedly crept in,nd the author would grea.tly appreciate notations of any ofhese which may come to the reader's attention, with a view0 their correction in later reprints or editions of the book.A large amount of time and labor was involved in the prepara-

ion of these tables, inasmuch as it was necessary to collectata from

many widely scattered sources. The scope of therst issue, therefore, is rather more Umited than originallylanned, but if the demand for the pubUcation justifies it, thecope will be extended in future issues.The author wishes to express his appreciation to the many

lends who assisted in checking problems, reading the manu-3ript and proof, and giving much valuable criticism anddvice.

Thomas J. Sullivan.De Pub, III.March 1, 1918.


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CONTENTSPagb

Preface v

NTERNATIONAIi ATOMIC WeIOHTS xii

Ipecific Gravitt 1Definition of 1More Common Methods of Determining 1Corrections to be Applied 2Conversion of Basis 3

Itdrometebs 6Types 5Classes 5Manipulation 5

American Standard BAtjM:^ Hydrometer 8Specific Gravities Corresponding to Degrees Baum6 11Degrees Baum^ Corresponding to Si)ecificGravities 16

Twaddle Hydrometer 20SpecificGravities Corresponding to Degrees Twaddle 21

fombnclature of Sulphuric Acid 22Formulas for Use in Sulphuric Acid Calculations 24)e8criftion of Methods Employed in Preparing the Tables ofSpecific Gravity of Sulphuric Acid, Nitric Acid, and Hydrochlo-ic

Acid, Adopted by the Manufacturing Chemists' Associationop the United States 27

Nitric Acid Table 49Hydrochloric Acid Table 51Sulphuric Acid Table 64

iuLPHURic Acid 94-100 Per Cent. HjS04 60^PHURic Acid 0**B .-100 Per Cent HsSOi 61te HURic Acid 50*'-62*' B 68^JMiNG Sulphuric Acid 71

Per Cent. Free SO. as Units 74Per Cent. Total SO. as Units 76Equivalent Per Cent. 100 Per Cent. HsSOi as Units 79

SpecificGravity Test Sulphuric Acid 76.07-82.6 Per Cent. S0 81ix


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X CONTENTSPag

SuiiPHTTRic Acid Per Cent SOs Correbpondinq to Even Percent- IAGES HjSO* i

Sulphuric Acid Per Cent H2SO4 Corresponding to EIven Per-entagesSOj 81

Acid Calculations, Use of Specific Gravity Tables, Estimating iStocks, etc 81

Dilution and Concentration of Sulphuric Acid to form SolutionsOF Any Desired Strength 8{

Table for Mixing 59 * Baum6Table for Mixing 60^ Baum6Table for Mixing 66^ Baum6 9

Formation of Mixtures of Sulphuric and Nitric Acids of DefiniteComposition (So-called Mixed Acid)

BoiuNG Points Sulphuric AcidMelting Points Sulphuric AcidTension of Aqxteous Vapor Sulphuric AcidStrength for Equilibrium with Atmospheric Moisture ....Preparation of the Mono-hydratePounds Sulphuric Acid Obtainable from 100 Poxtnds Sulphur

. .

Pounds Sulphuric Acid Obtainable from 100 Pounds SOj ....Pounds Sulphur Required to Make 100 Pounds Sulphuric Acid

.

The Quantitative Estimation of Sulphur Dioxide in Burner GasTest for Total Acids in Burner GasCalculating the Percentage SO2 Converted to SOg When the

SOt in the Burner and Exit Gases is Known as Used in theContact Process

TableTheoretical Composition of Dry Gas from the Roasting of

Metallic Sulphides, .

Theoretical Composition of Dry Gas from the Combustion of Sul-hur

Qualitative Tests Sulphuric AcidNitrogen Acids Selenium ^Lead Iron and Arsenic

Quantitative Analysis op Sulphuric AcidQuantitative Determination of Lead, Iron and Zinc in Sulphuric

AcidThe Analysis OF Mixed Acid AND NiTRATBD-SuLPHURic Acid ....Calibration op Storage Tanks and Tank CarsMathematical Table Circumference and Area of Circles,Squares, Cubes, Square and Cube Roots

Decimals OF A Foot for Each K4 ^^CH


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CONTENTS xiPaqb

Decimals of an Inch fob Each H4 ^77Selting Rules 177^Nn-FBEBZINO LlQUIDS FOR PRESSURE AND SUCTION GaGES 178

Table 179^LANQEB AND FlANGED FiTTINGS 180

Names of Fittings 182Templates for Drillingtandard and Low Pressure Flanged Valves

and Fittings 183General Dimensions of Standard Flanged Fittings Straight

Sizes 184General Dimensions of Standard Reducing Tees and Crosses ... 186General Dimensions of Standard Reducing Laterals 187General Dimensions of ^tra Heavy Flanged Fittings Straight

Sizes 188General Dimensions of Extra Heavy Reducing Tees and Crosses . .190General Dimensions of Extra Heavy Reducing Laterals 191Templates for DrillingExtra Heavy Flanged Valves and Fittings . 192Weight of Cast-iron Flanged Fittings 193

Dast-Iron Pipe 194Nominal Weight of Cast-iron Pipe Without Flanges 194Standard Cast-iron Pipe Standard Dimensions 195

Brought Iron and Steel Pipe 197Standard Wrought Iron and Steel Pipe 197Extra Strong Wrought Iron and Steel Pipe . . . . ' 199Double Extra Strong Wrought Iron and Steel Pipe 200Standard Outside Diameter (O. D.) Steel Pipe 201

Brewed Fittings 202Standard Screwed Fittings 202Extra Heavy Screwed Fittings 203

^ERICAN BrIGGB STANDARD FOR TaPER AND STRAIGHT PiPE AND LoCK-NUT Threads 204

:-eadPipe 206^heet Lead 207^ANDARD 9'' AND 9 SeRIES BrICK ShAPES 208Fibre Rope Knots and Hitches and How to Make Them .... 210[J.S. CusTOMART Weights and Measures 213Metric Measures 214Bquivalentb of Metric and Customary (U. S.) Weights andMeasures 216

i 3oMPARisoN of Thermometric Scales 219Fahrenheit degrees as units 219


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xii CONTENTS

Paqi

Centigrade Degrees as Units 220Water 221

Density and VolumeDensity of Solutions op Sulphuric Acid 222Temperature Corrections to Per Cent of Sulphuric Acid Deter-ined

BT THE Hydrometer 224Specific Gravity of Sulphuric Acid 225Specific Gravity of Fuming Sulphuric Acid 233

Index 235


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INTERNATIONAL ATOMIC WEIGHTS xiu

International Atomic Weights, 1917*Symbol Atomicweight Symbol Atomicweight

Juminum..kntunony.. .

LTgonoisenicteuiumiismuth

....loronIromine..

. .

Sadmium. . .iffisiumialcium.

. . .arbonJeriumJhlorlneIhromium

. .iobaltblumbium.

.Jopper^ysproaiumIrbiumluropium . .ludrineradoliniutn

. .ralliumlermanium

. .rlucinum. . . .bid

ielium[olmium. . . .[ydrogenidium)dineidiumt)iijyptoninthanum.

.2adithiumitecium. . . .[agnesium

.Manganese. .tercury[olybdenum

AlSbAAsBaBiBBrCdCsCaCCeCICrCoCbCuDyErEuFGdGaGeGlAuHeHoHInIIrFeKrLaPbLiLuMgMnHgMo

27.1120.239.8874.96

137.37208.011.079.92

112.40132.8140.0712.005

140.2535.4662.068.9793.163.67

162.6167.7162.019.0

157.369.972.59.1

197.24.00

5008

1631114.8126.92193.165.8482.92

139.0207

.20

6.94175.024.3264.93

200.696.0

NeodyiniumNeonNickelNiton (radium em-nation)NitrogenOsmiumOxygenPalladiumPhosphorusPlatinumPotassiumPraseodymiumRadiumRhodiumRubidiumRutheniumSamarium

,

ScandiumSelenium..;

SiliconSilverSodiumStrontiumSulphurTantalumTelluriumTerbiumThalliumThoriumThuliumTinTitaniumTungstenUraniumVanadiumXenonYtterbium (Neoyt-terbium)Yttrium

ZincZirconium

NdNeNiNtNOsOPdPPtKPrRaRhRbRuSaScSeSiAgNaSrSTaTeTbTlThTmSnTiWUVXeYbYtZnZr

144.320.268.68

222.414.01

190.916.00

106.731.04

196.239.10

140.9226.0102.986.45101.7160.444.179.228.3

107.88

23.0087.6332.06

181.5127.5169.2204.0232.4168.5118.748.1

184.0238.251.0

130.2173.688.766.3790.6

* On account of the difficultiesof correspondence between its members due to the war, theterDational Committee on Atomic Weights has decided to make no full report for 1918.^ou^^ha good number of new determinations have been published during the past year,ne of them seem to demand any immediate change in the table for 1917. That table,uiere-^ may stand as officialduring the year 1918.~F. W. Clabk, Chairman.


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SULPHURIC ACID HANDBOOKSPECIFIC GRAVITY

Definition of the Term ''Specificravity of a LiquidThe density of a liquidis defined as the weight of a unit volume.The specificgravity, or the synonymous term, relative density,the ratio of the density of the liquidin question,referred to themsity of some substance which is taken as unity. The standardibstance employed is water at its maximum density (4 C. or).2^.).ilore Common Methods of Determining the SpecificGravity of Liquids1. Pycnometer. Here we have vessels of unknown volume,at either having a mark on the neck, or having glassstopperith a capillaryhole. Thus the pycnometers are made to hold}nstant volumes. Constant temperature is obtained by the aidI a bath of constant temperature. For use in a determinationle pycnometer is weighed empty, filled,with water, and filledith the liquidunder consideration. The weight of the pycnom-;er full of water minus the weight of the empty pycnometer isjualto the weight of the water it will hold. This weight, com-ired to the weight of the liquidthat the pycnometer will hold,ives us the specificgravity of the liquid.2. Mohr, Westphal, Sartorius, Specific-gravity Balances. Inle balances the right-handhalf of the beam is divided into ten|ual parts from the fulcrum to the point of suspension at theid of the beam. Suspended from this end of the beam is thelummet while a weight at the other end acts as a counterbalance,rhen the plummet is immersed in water at 4 C., the equilibriumf the balance is destroyed by the buoyancy of the water. Toiljusthe equilibrium, a weight equal to this force and in gramsjual to the weight of the volume of water displaced (which isijualto the volume of the plummet) is hung from the point of

1


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2 SULPHURIC ACID HANDBOOK

suspension.This weight is known as the unit weight and Lcalled a rider. Other riders weighingrespectively.1,0.01,O.OOlof the weightof this rider constitute the set of weightsused witlithese balances. With their aid the densityof a liquidcan bedirectlyead off from the balance beam.

3. Hydrometers. These instruments consist of a spindleshaped float,with a cylindricaleck containinga scale. Thejare weighted at their lower end, thus bringingthe center olgravityvery far down, and insuringn uprightpositionwhenfloating.They depend upon the principlehat a body will sinkin a liquidimtil enough liquidhas been displaced,o that theweightof the displacediquidequalsthe weightof the body.

The weightand volume are so adjusted,hat the instrumesinks to the lower mark on its neck in the heaviest liquidto betested by it,and to the highestmark on its neck in the lightestliquido be tested by it. As the densityof a liquidchanges witithe temperature,the liquidshould alwaysbe at the temperatunat which the hydrometer was calibrated or proper correctioimade.

Corrections to be Applied in SpecificGravity DeterminationsTo obtain the true specificravityof substances,heir densitid

at 4^C., and in vacuo ^ must be compared with the density clwater at 4 C.,in vacuo.

For technical use, specificravityis frequentlyetermined alany convenient temperature, and referred to water, of eithefthat same temperature, or to water at 4^C.,the weight in aiibeingtaken as a basis.

In purelyscientificcalculations,ater is taken as standard a|4^C.,while in commercial laboratories the standard is often i^the neighborhoodof 15.56 C.,consequentlyspecificgravitieidetermined by these standards do not agree. As the tempersture of water increases from 4 C.,itexpands. The weightbeinlconstant,with increase of volume, the densityis lowered. Iithe case of water this increase of volume with riseof temperatuiis not uniform,but has been determined with great care. Kno^ing the relative densityof water at various temperatures,th|


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SULPHURIC ACID HANDBOOK

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HYDROMETERS 5

HYDROMETERSThere are two types of hydrometers, namely, hydrometers

roper, and hydrometers which are combined with thermometers,illedthermo-hydrometers.There are four classes of hydrometers:1. Density hydrometers, indicatingdensity of a specified\mdj at a specifiedtemperatm'e, in specifiednits.2. Specific-gravityydrometers, indicatinghe specificravity

relative densityof a specifiediquid,t a specifiedemperature,terms of water at a specifiedtemperature as unity.3. Per cent, hydrometers, indicating,t a specifiedtempera-ire, the percentage of a substance in a mixture or solution.4. Arbitrary scale hydrometers, concentration or strength ofspecifiedliquid referred to an arbitrarilydefined scale at alecifiedtemperature (Baum6 hydrometer, Twaddle hydrometer,c).

Manipulation of Hydrometers^Hydrometers are seldom used for the greatestaccuracy, as theual conditions under which they are used precludesuch specialstnipulationand exact observation as are necessary to obtain^h precision. It is, nevertheless,important that they beDurately graduated to avoid as far as possible,he use of in-ximental corrections,nd to obtain this result it isnecessary toiploy certain precautionsand methods in standardizingtheseitruments.The methods of manipulationdescribed below are, in general,3 ones employed at this Bureau in testinghydrometers anduld be followed by the maker or user to a degree dependingthe accuracy required.Observing. The hydrometer should be clean,dry,and at thenperature of the liquidbefore immersing to make a reading.The liquid in which the observation is made should be con-ed

in a clear,smooth glassvessel of suitable size and shape.U. S. Bureau of Standards,Circular No. 16,4th edition,Feb. 23, 1916.


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By means of the stirrer which reaches to the bottom of 1|vessel,the liquidshould be thoroughlymixed.

The hydrometer is slowlyimmersed in the liquidslightlyyond the point where it floats naturallyand then allowed Ifloatfreely. i

The scale readingshould not be made imtil the liquidai|hydrometer are free from air bubbles and at rest. i

In reading.the hydrometer scale the eye is placedslightlylow the planeof the surface of the test liquid;t is raised slountil the surface,een as an ellipse,ecomes a straightine,pointwhere this line cuts the hydrometer scale should be tas the readingof the hydrometer.

In readingthe thermometer scale,rrors of parallaxre avoiby so placingthe eye that near the end of the mercury colthe portionson either side of the stem and that seen throughcapillaryppear to lie in a straightline. The line of sightthen normal to the stem.

Note : Accordingo the Bureau of Standards,then, the pointA (seebelow) not the point B is the one to be noted as the reading.Influence of Temperature.

order that a hydrometer mayrectlyindicate the densityor strenof a specifiedliquid,it is essen

^^g that the liquidbe uniform thro==- out and at the standard temperatzEEiE: To insure uniformityin the liqEEE. stirringis required shortly beW

making the observation. This 4ring should be completeand mayi

well accomplishedby a perforateddis^ or spiralat the end drod longenough to reach the bottom of the vessel. Motion 'this stirrer from top to bottom serves to disperselayersof ^liquidof different density.

The liquidshould be at nearlythe temperature of the surroiflingatmosphere,s otberwi3e its temperaturewill be chann

SL

= 60

^


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HYDROMETERS 7

luringhe observation,causingnot only differences in density)utalso doubt as to the actual temperature. When the tem-lerature at which the hydrometer is observed differs from thetandard temperature of the instrument,the readingis not trulyhedensityaccordingto the basis of the instrument or the quahtyfthe liquidaccording to per cent, or arbitraryscale,but a figurerhichdiffers from the normal reading by an amount dependingh the difference in temperature and on the relative thermal ex-ftasions of the instrument and the particularliquid.If the latter propertiesare known, tables of corrections forjmperature may be prepared for use with hydrometers atarious temperatures. Such tables should be used with cautionlidonly for approximate results when the temperature differsluch from the standard temperature or from the temperature:the surrounding air.Influence of Surface Tension. Surface-tension effects on hy-ometer observations are a consequence of the downward forcelerted on the stem by the curved surface or meniscus, which)es about the stem, and affects the depth of immersion andDsequent scale reading.Because a hydrometer will indicate differentlyn two liquidsfvingthe same densitybut different surface tension,and sincerface tension is a specificroperty of liquids,t is necessary topcifythe liquidfor which a hydrometer is intended.AJthough hydrometers of equivalentdimensions may be com-red, without error, in a liquiddifferingn surface tension from3 specifiedliquid,omparisons of dissimilar instruments in suchiquid must be corrected for the effect of the surface tension,[n many liquidsspontaneous changesin surface tension occurB to the formation of surface films of impurities,hich mayne from the apparatus, the liquid,r the air.Errors from this cause are avoided either by the use of liquidsb subject to such changes,which,however, requirecorrectionthe results by calculation,r by the purificationf the surfaceoverflowing immediately before making the observation.


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8 SULPHURIC ACID HANDBOOKThis lattermethod isemployed at this Bureau for testingydrometers in sulphuric-acidsolutions and alcohol solutions,and iaccomplished by causingthe liquidto overflow from the part athe apparatus in which the hydrometer is immersed by a smalrapidlyrotatingpropellerwhich serves also to stir the liquid.

Cleanliness. The accuracy of hydrometer observations depends,in many cases, upon the cleanliness of the instruments aiMof the liquidsin which the observations are made.

In order that readingsshall be uniform and reproducible,thsurface of the hydrometers,and especiallyf the stem, must bclean,so that the liquidwill rise uniformly and merge into aimperceptiblefilm on the stem.

The readiness with which this condition is fulfilleddependsomewhat upon the character of the liquid,ertain liquids,sueas mineral oils and strong alcoholic mixture,adhere to the steivery readily,while with weak aqueous solutions of sugar, saltacids,and alcohol,scrupulous cleaningof the stem is requirein order to secure the normal condition.

Before being tested,hydrometers are thoroughlywashed |soap and water, rinsed,and dried by wiping with a clean lin^cloth.

If to be used in aqueous solutions which do not adhere readilthe stems are dipped into strong alcohol and immediately veipdry with a soft,clean,linen cloth.

AMERICAN STANDARD BAUMB HYDROMETER(LiquidsHeavier than Water)

The Manufacturing Chemists' Association of the United Statand the United States Bureau of Standards have adoptedBaum6 scale based on the followingrelation 'to specificgravit

145Degrees Baum^ = 145 Specificgravityat ^tjoF-

or

bpecinc gravity at ^t^F. =60 ' 145 degreesBauin6


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BAUM6 HYDROMETERS 9

The followinghistoryof the Baum^ scale istaken from Circular^o, 59 issued by the United States Bureau of Standards,April5,1916:

The relation between specificravity and Baum6 degreesrepresentedby^he formulas given was adopted by this Bureau in 1904, when it firsttook up'.hequestionof testinghydrometers. At that time every important manu-'acturer of Baum6 hydrometers in the United States was using this relationis the basis of these instruments,r at least such was their claim.

''The origin and early historyof the Baum6 scales has been admirablytreated by Prof. C. F. Chandler in a paper read before the National Academy3f Sciences at Philadelphiain 1881. As this paper may not be readilyavailable to some who are interested in the matter, it may be well to includelierea part of the material prepared by Prof. Chandler.

''The Baum6 scale was first proposed and used by Antoine Baum^,ft French chemist, in 1768, and from this beginning have come dififerentBaum6 scales that have been prepared since that time. The directionsp^ivenby Baum6 for reproducing his scale were firstpublished in L'Avant in1768, and though simple,are not specific,nd the conditions assumed are noteasilyreproducible. It is not strange, therefore,that differences soon ap-eared

between the Baum6 scales as set up by dififerentobservers. Thatthis divergence did actually occur is well shown by the large number ofBaum6 scales that have been used. Prof. Chandler found 23 dififerentscales for liquidsheavier than water.

Baum^'s directions for settingup his scale state that for the hydrometerscale for liquidsheavier than water he used a solution of sodium chloride(common table salt) containing 15 parts of salt by weight in 85 parts ofwater by weight. He described the salt as being 'very pure'and 'verydry'and states that the. experiments were carried out in a cellar in which thetemperature was 10 Reaumur, equivalent to 12.5*'C. or 54.5**F.

The point to which the hydrometer sank in the 15 per cent, salt solu-ionwas marked 15**,nd the point to which it sank in distilled water at the

same temperature was marked 0 . The space between these two pointswas divided into 15 equal parts or degrees,and divisions of the same lengthwere extended beyond the 15**point.Other makers of Baum6 hydrometers soon began to deviate from the pro-edure

outlined by Baum^, the deviations being,no doubt, partlyaccidentaland partly intentional,and in course of time, as already pointedout, manydififerentBaum6 scales were in use.

This condition of afifairs led to great confusion in the use of theBaum^ scale.


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10 SULPHURIC ACID HANDBOOK From a consideration of the variations that occurred it was soon evident

that some means- of definingand reproducing the scale more exactly than(70uld be done by the simple rules given by Baum^ should, if possible,befound. This means was readilyprovided by assuming that a fixed relationshould exist between the Baum6 scale and the specific-gravitycale at somedefinite temperature, and in terms of some definite unit. When this relationis expressed in mathematical terms in the form of an equation, then theBaumjd scale is fixed beyond all questionsof doubt. At the present time allBaum6 scales in use are based on such an assumed relation,and the differ-nces

existingbetween them arise from dififerencesin the assumed relationor ^modulus' on which the various scales are based, and the standard tem-erature

at which the instruments are intended to be correct.''If a definite modulus is adopted, then the degrees Baum6 correspondingto any given specificgravity,or the specificravity corresponding to anygiven degree Baum6 may be calculated;or if the specificgravity andcorresponding degree Baum6 at any point of the scale are known, then themodulus can be determined and the complete Baum6 scale calculated fromthis singlepoint.Let 8 specificravity.d degrees Baum^.

m s modulus.Then for liquidsheavier than water :

m8

m da = w

8dam = 8-1

At the time the Bureau of Standards was contemplatingtakingup thework of standardizinghydrometers (1904),diligentinquiry was made of themore important American manufacturers of hydrometers as to the Baum^scales used by them. Without exceptionthey repliedthat they were usingthe modulus 145 for liquidsheavier than water. This scale,the ''AmericanStandard,''as therefore adopted by the Bureau of Standards and hasbeen in use ever since.

There having been no objection or protest from any manufacturer oruser of Baum^ hydrometers at the time the scale was adopted by the Bureau,it was assumed that they were entirelysatisfactoryo the American tradeand were in universal use.''


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Specific Gravities at 60^ /15.56^60** \15.56'6 /Degrees Baum {Continued)

C. I Corresponding to


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BAUME HYDROMETERS 13

Specific Gravities at 60;60* ,/15.56 \ CORRB8PONDINO TO

Degrees Baum^ (Continued)


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baum6 hydrometers 15

Specific Gravitibs at 60*60*** \15.56**Degrees Baum (Conduded)

CORRESPONDINQ TO


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37/268

BAUME HYDROMETERS 17

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38/268


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39/268


40/268


TWADDLE HYDROMETER

(Generally used in England)Methods of Converting Specific Gravity to Degrees Twaddle

1. Let X = degrees Twaddle.y = specific gravity.

10002/ - 1000^== 5

2. Or X = 200 {y - 1).

3. This method may be used for any value below 2.000. Movethe decimal point two figures to the right, striking off the firstfigure and multiplying the remainder by 2.

Methods of Converting Degrees Twaddle to Specific Gravity

1. Let X = specific gravity.y = degrees Twaddle.

^

by + 1000^ 1000

^ ^^^ = 2^ + 1a

The degrees in Twaddle's hydrometer bear a direct relation-hipto the specific gravity, the basis of the system being plain

and unmistakable, since every degree is equal to a difference inspecific gravity of 0.005.


41/268

TWADDLE HYDROMETER 21


42/268

22\

SULPHURIC ACID HANDBOOK

NOMENCLATURE OF SULPHURIC ACID

Sulphuricacid shows a definite relation between the specificgravityand strengthup to 93.19 per cent. H2SO4. As itis mucheasier to determine the specificravitythan the strength,acidsweaker than 93.19 per cent, are nearlyalways spoken of and soldas beingof so many degreesBaum^, the Baum6 hydrometer beingthe instrument generallysed for determiningthe specificravity.The principalstrengthsof such acids are :

In 1882 the Manufacturing Chemists' Association of theUnited States agreed on a set of values for Baum6 degrees andtheir H2SO4 equivalents. In 1904 the Association adopted thetable of Ferguson and Talbot. The H2SO4 equivalentsshow aslightchange from the table of 1882 and those values have beenused in this country ever since. In Germany especially,ndquite generallyon the continent,a different set of values forBaum6 degreesis used in which all have highervalues in specificgravityand H2SO4 than those used here. For instance 66**B6.here correspondsto 93.19 per cent. H2SO4 and in Germany to98 per cent.

The 66**acid is also known as oilof vitriol (O.V.)and strengthsof weaker acids are sometimes spoken of as so many per cent.0. v., a 60 B6. acid containing77.67 per cent. H2SO4 beingcalled 83.35 per cent. O. V.

77.67 X log93.19 = 83.35


43/268

NOMENCLATURE OF SULPHURIC ACID 23

This,however, is not very common. In reportingtotal pro-uctionor uses of sulphuric acid it is frequentlystated as being

equivalentto a certain quantityof acid of 60**or 60^ or some otherstandard strength,the total amount of H2SO4 being the same asthat contained in the stated quantity of the stated strength.Productions are also often reported as tons of SOj.

When an acid becomes stronger than 93.19 per cent. H2SO4,to speak of it in terms of specificgravityor degrees Baum wouldbe fallaciousas 94.5 per cent, acid has practicallythe same specificgravitys 100 per cent. Acids between 93.19 and 100 per cent.are spoken of as so many per cent, sulphuric acid;100 per cent,acid being commonly called the mono-hydrate. This contains100 per cent. H2SO4 (81.63 per cent. S0 ).SO3 dissolves in the mono-hydrate giving fuming acid or

oleum. It is called fuming acid because the SOs escapes, form-ngwhite fumes, when exposed to the air. Oleum is the German

name which has been used extensivelyin this country, since thefirstpracticalmethods of making it were German and the Germannomenclature was frequently adopted here. It is also known inGermany as Nordhausen Oil of Vitriol.There are three ways of stating the strength of fuming acid:1. The per cent, of free (dissolved)SOs.2. The per cent, of total SOs.3. The equivalent per cent. 100 per cent. H2SO4. That is the

per cent, of 100 per cent. H2SO4 it would make ifsuflBcient waterwere added to combine with all the free SOs.For instance an acid containing 20 per cent, free SOs would

contain a total of 85.30 per cent. SO3, and actual H2SO4 contentof80 per cent, and would make 104.49 per cent. H2SO4 ifsufficientwater were added to combine with all the free SO3. It might,therefore,e called 20 per cent.,85.30 per cent, or 104.49 per cent.Mixed acid is the technical term for a mixture of strong sul-

phnricacid and nitric acid.


44/268


FORMULAS FOR USE IN SULPHURIC -ACID CALCULATIONS

(By non-fuming acid is meant all strengths under 81.63 per cent. SOs)(By fuming acid is meant all strengthsover 81.63 per cent. SOs)

The followingfactors were calculated from molecular weights:SOs 80.06

SO3 80.06To Calculate Per Cent. SOa Non-fuming Add

Per cent. H2SO4 X 0.8163or Per cent. H2SO4 -^ 1.2250

To Calculaie Per Cent H2SO4 Non-fuming Acid Per cent. SO3 -^ 0.8163

or Per cent. SO3 X 1.2250To Calculate Per Cent. Free H2O Non-fuming Add

100 - per cent. H2SO4To Calculale Per Cent. Combined H2O Non-fuming Add-

Per cent. H2SO4 per cent. SOsor Per cent. H2SO4 X 0.1837or Per cent. SOs X 0.2250


45/268

SULPHURIC-ACID CALCULATIONS 25

To Calculate Per Cent. Combined H2O Fuming Acid Per cent. H2SO4X 0.1837

or 100 per cent, total SO3or Per cent, combined SO3 X 0.2260

To Calculate Per Cent. H2SO4 Fuming Add 98.076 (100 ~ per cent, total SOs)

18.018

or 100 per cent, free SOsor Per cent, combined H2O X 5.4438orPer cent, combined H2O + (4.4438X per cent, combined H2O)

To Calculate Equivalent100 Per Cent, H2SO4 Fuming Acid Per cent, total SOs -^ 0.8163

or Per cent, total SO3 X 1.2250

To Calculaie Per Cent. Combined SOs Fuming Acid 80.06 (100 - per cent, free SO3)

98.076or Per cent. H2SO4 X 0.8163or Per cent, combined H2O X 4.4438or Per cent, total SO3 per cent, free SOs

To Calculate Per Cent. Free SOs Fuming Add (Per cent, total SO3 X 98.076) - 8006

18.016or (Per cent, total SOs X 5.4438) - 444.38or (Per cent, total SO3 - 81.63)5.4438or Per cent, total SO3 (percent, combined H2O X 4.4438)or Per cent, total SOs per cent, combined SOsor 100 Per cent, H2SO4


46/268


To Calculate Per Cent. Total SO3 Fuming Add (Per cent, free SOs X 18.016)+ 8006

98.076or (Per cent. free.SO3 X 0.1837) + 81.63or 0.8163 (100 - per cent, free SO3) + per cent, free SOsor Equivalent per cent. 100 per cent. H2SO4 X 0.8163or Per cent, free SO3 + per cent, combined SOs

To Calculate Weight per Cubic Foot Add

Specificgravityat ^F. (iTTftoC.X weight per cubic footwater at 60 F. (62.37lb.)

To Calculate Weight SO3 per Cubic Foot(Weight of acid per cubic foot X per cent. SO3) -5- 100)

To Calculate the Equivalent Per Cent, and Weight of OneStrengthAdd af Compared to Another

The equivalentper cent, in 66 B^. (93.19per cent. H2SO4) ofan acid of 60 B^. (77.67per cent. H2SO4) is:

^^ X 100 = 83.35 per cent. 66 B6.and as 60 B^. correspondsto 1.7059 specificgravity,the poundsof 66 B6. equivalentto 1 cu. ft. of 60''B^. is:

J^ X 1.7059 X 62.37 = 88.68 lb. 66^B6.Note. While ascertainingequivalents of non-fuming acid, strengths

used for the calculations can either be taken as per cent. SOs or of per cent.H2SO4.

If calculatingfuming-acid equivalents,strengthsshould be used in termsof total per cent. SO3 unless expressed in the equivalentper cent, of 100 percent. H2SO4.


47/268


48/268


The acids and ammonia used were the pm'est obtainable e.p.,and were carefullyxamined for impuritiesand purifiedwhennecessary. The impuritiesin commercial products are such avariable quantity and, as their purityis becoming more pro-ounced

as manufacturingprocesses improve, many substancesmade on a largescale beingnearly c.p., it was deemed that thetables would have more practicalvalue if they were based uponc.p. compounds. As to any scientificmerit they may possess, itis needless to say that such a positivebasis to which they canalways be referred is an essential.

All of the analyticalnd specific-gravityeterminations,de-erminof the coefficient of expansion (or allowance for

temperature),determination of boilingpoints,as well as all cal-ulatiand clericalwork, were performed by two experienced

men working independently.SPECIFIC-GRAVITY DETERMINATIONS

All specific-gravityeterminations were taken at 60**F.,om-aredwith water at 60 F. The work was done in winter and no

account was taken of differences of atmospheric pressure oitemperature,which averaged about 760 mm. and 65**F.

The apparatus used in this work was a 50-c.c. Geissler picnonHeter having a capillaryside-arm tube fitted with a glasscap, inthe top of which was a small hole which allowed the liquidtoexpand without looseningthe thermometer or cap, at the sam^time preventing loss while weighing. The thermometer, whichwas ground to fit the neck of the bottle,as graduatedto J'^ F.and readable to Ks^F., and was frequentlychecked againstastandard thermometer.

Before making a determination the water content of the bottfewas firstaccuratelydetermined and checked from time to timeduring a series of determinations. To obtain the water content,the bottle together with the thermometer and glass cap wericarefullycleaned, dried and weighed. (The accuracy of thflbalance and weights were systematicallychecked against a


49/268

COEFFICIENT OF EXPANSION 29

standard set of weights.) The bottle was then filledwith freshly-distilledwater at 55 -57**F.,nd the thermometer tightlyin-erted.

As the temperature slowly rose, the water expandedthroughthe capillaryide arm. When the thermometer regis-ered60T., the last drop was removed from the top of the capil-ary,the tube capped and the whole weighed. This weight,less

the tare obtained above, was taken as the water content of thebottleat 60**P. Check determinations agreed within 0.002 gram,or lessthan 0.00005 specificgravity. Distilled water freed fromcarbon dioxide by boiling,nd coolingin a closed vessel,ave thesame water content as the ordinary distilled water which wasused throughout the work. This water was free from chlorideand residue upon evaporation.

In determining the specificravityof liquids,he weight of theliquidontained by the bottle at 60**F. was obtained as above.This weight, divided by the water content, equals the specificftgravity.It was thought that the temperature of the liquidin the bottle

might vary in diflferent parts and the whole not have the sametemperature as registeredby the thermometer in the center ofthe bottle. To ascertain the facts in the case a beaker was filledwith water below the temperature of the room, and a thermom-ter

placed in the center of the beaker showed the same tempera-ureas those placed near the sides,the temperature risinguni-ormly

throughout the liquid.COEFFICIENT OF EXPANSION

The correction for temperature was found by allowing thetquidto slowly expand, and when the temperature had risen8 ~10**F.,he tube was wiped off and capped, and the apparatusagainweighed. Another weight was taken at a stillhighertem-erature,

and from these results the difference in specificravityfor1*T. and the number of degreescorrespondingto 1**B^. werecalculated. To determine how much the expansion of the pic-nometer affected the specific-gravityeterminations at different


50/268

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51/268

COEFFICIENT OF EXPANSION 31

About 200 grams of sodium bicarbonate were washed in afunnel having a porcelainplateuntil entirelyfree from chloride.It was then dried at lOO^^C,protected from acid gases, finelyground, and kept in a sealed bottle until used. About 20 gramsof bicarbonate thus prepared was heated in a platinum dish ata moderate red heat, until the weight was constant, and then5 grams was quicklyand accuratelyweighed for analysis. Ourattention was directed to the method of heatingsodium carbon-te,

for,in standardizing,arious results were obtained depend-ngon the temperature of ignition,the highest temperaturegiving the greatest alkalinity,r about 0.09 per cent, greater

than the lowest. It remained to be proved whether the high orlow result was correct, and whether in heating to the highertemperature (redheat over a Bunsen flame)water was givenoff,or whether the loss in weight was due to a decomposition ofsodium carbonate into sodium oxide and carbon dioxide.

In referringto the Uterature several references were foundupon the ignitionof sodium carbonate. MendeleeflF,ol. I, p.525, in quoting the work of Pickering,says: ''When sodiumcarbonate is fused about 1 per cent, of carbon dioxide is disen-aged.'*

In Lunge's Untersuchungs Methoden, vol. I,p. 83,reference is made to an articlein Zeitschr. /.Angew. Chem., 1897,p. 522, by Lunge, in which he says that soda intended for thestandardization of acids must not be heated higher than 300^C.(572**F.) iid if the heatingis carried on at this temperature fora suflKcientlengthof time,one may be sure that neither bicarbon-te

nor water is left behind, and yet no sodium oxide has beenformed as may happen if the heatingis carried to a low red heat.

Sodium Carbonate ( ). A portionof the washed and driedbicarbonate was carefullyheated in a platinum crucible withoccasional stirringt 572 F. to constant weight,and immediatelyanalyzed.

Ammomum Sulphate. Ten grams of the standard acid (tobehereinafter described)were quicklyand accuratelyweighed in asmall glassweighingtube,avoidingabsorptionof moisture from


52/268


the atmosphere. After rinsingthe sample into a largeplatinunidish,it was made slightlyammoniacal with ammonia that hadbeen freshlydistilled to free it from silica. During evaporatiopon the steam bath, the dish was kept covered by a largefunneland protected from acid fumeis. Ammonia was added from timeto time, as it was found that the salt became acid on evaporation.After evaporation the dish was dried in an air bath to constantweight at 230^F. i

Sulphuric Acid (100 Pw Cent H2SO4). In reviewing thework of Pickering {Jour.Chem. Soc, 1890) it occurred to us thaiit would be possibleto make some pure 100 per cent. sulphuri ^acid,and that the anal3rsisf this would serve as a suitable checkon our other methods. Pickering has shown that the curve oithe melting point of sulphuricacid near 100 per cent, reaches flmaximum at 100 per cent. Therefore,by startingwith an acidslightlyless than 100 per cent, and another slightlymore thari100 per cent., a point should be reached in recrystalUzingherithe successive crops of crystalsobtained from both acids shouldshow the same per cent, sulphuricacid. This was actuallythdcase. I

Starting with 2 liters of chemicallypure sulphuricacid, purdredistilled sulphuricanhydride was added until,on analysis,thestrength was 99.8 per cent. The bottle was shaken during crys-allizatio

so as to obtain small crystals,and when the bottlewas half full of crystalsthe mother liquorwas drained off througha porcelainplate fitted over the mouth of the bottle and havinga glasstube passingthrough its center to the bottom of the bottlethrough which air dried with strong sulphuricacid was admitted,when the bottle was inverted. By draining the crystals forseveral hours at a temperature slightlybove the melting point,the mother liquor was entirelyremoved. These crystals werethen melted and recrystallized,nd drained as described above.The crystals thus contained were melted, recrystallizedanddrained,the final crystalsbeing melted and kept in a sealed


53/268

COEFFICIENT OF EXPANSION 33K)ttle until analyzed. Two litersof acid were prepared,analyz-ag 100.1 per cent, sulphuricacid. From this the standard wasprepared in exactlythe same manner as in the case of acid analyz-Qg 99.8 per cent, sulphiuicacid.Sulphtiric Anhydride. ^Another method used as a check on

ur standard was the titration of sulphuricacid formed by the4ldition of water to 100 per cent, sulphuricanhydride. To dohis required especialare first,o obtain a sample of sulphuricjihydride free from water, and, after obtainingit,to mix it withrater without loss of anhydride. The plan adopted was asolio w^s :Fuming sulphuricacid containing40 per cent, free SOj was

Ustilled at a low temperature into a long-necked flask fittingightly over the deliverytube of the retort. A few crystalsofK tassium permanganate were added to oxidize any sulphurLioxide present. The first 25 c.c. of the distillatewere rejected.kbout 200 c.c. were distilledover. Then this 200 c.c. was redis-illed, rejectingthe first few cubic centimeters and collectingkbout 100 c.c. in an ordinarydistillinglask,o the deliveryuberf which was sealed the open end of a test-tube,hich had beenIrawn out in the center,and bent at the constricted part, almostx a right angle,thus forminga receiver. As soon as the distilla-aon into the flask was completed the neck was sealed,thusnaking the whole apparatus air-tight.By warming the flaskDO 140**F. and coolingthe receiver,bout 20 grams of sulphuricixihydride were distilled over into the latter,hich was thenlealed at the constricted part having a slightacuum.

SulphanilicAcid. In lookingthrough the listof organicacidsfor one that would be suitable,ulphaniliccid was decided upon[ D. account of its beinga monobasic acid with a high molecularvireight,rystallizingithout water and drying without decompo-ition.

The so-called c.p. acid was recrystallizedhree times,finely ground, and dried in an air bath at 230 F. to constantweight.

3


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34 SULPHURIC ACID HANDBOOKANALYSIS OF STANDARDS

For the comparison of the above carefullyreparedcompoundsas standards 2 litersof c.p. sulphuricacid were used. This acidwas tested for impurities,ound to be practicallyfree,and waskept sealed when not in use, its percentage composition beingdetermined as follows:

Soditim Carbonate (a). Five grams of freshlyignitedsodiumcarbonate,prepared as above, were quicklyweighed out, and anamount of standard acid,slightlyn excess of the amount requiredfor neutralization was weighed in a small weighing tube andwashed into a flask containing the sodium carbonate. Afterboilingfor 15 min. to expelcarbon dioxide,the excess of sulphuricacid was titrated with N/2 sodium hydroxide,using phenolph-thalein as indicator. A short stem funnel was placedin the neckof the flask to prevent loss while boiling. Duplicate analysesofthe standard acid by this method gave 97.33-97.35 per cent, ofsulphuricacid.

Soditim Carbonate (b). Five grams sodium carbonate, pre-aredas above by heatingat 572**F. to constant weight,were used

in determining the strength of our standard acid. Observingexactlythe same conditions described above, we obtained 97.41-97.42 per cent, sulphuricacid.

Ammonium Sulphate. The ammonium sulphatedried to con-tantweight at 230 F.,s described above, was cooled in a desic-atorand quicklyweighed.

The salt was then dissolved in water and the small amount offree acid present, as indicated by methyl orange, was titratedwith N/3 sodium hydroxide. Adding an equivalentweight ofammonia to the weightabove,gave 97.41 per cent, as the strengthof the sulphuricacid. The d,mount of acid titrated was less than0.10 per cent, (withmethyl orange a sharp end pointisobtained).A dupUcate analysisgave 97.41 per cent, of sulphuricacid.

Sulphuric Acid (lOO Per Cent. H2SO4). About 6 grams ofacid,crystallizedrom 99.8 per cent, sulphuricacid,as describedabove,were introduced into the bottom of a small weighed tube|


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solution standardized on this basis to determine the strength ofour standard acid;it was found to be 97.41 per cent, of sulphuricacid.

Recapitulation of composition of standard sulphuric acid re*ferred to all the standards employed:

Per cent. Average

Sodium carbonate (A) Ignitedat low red heat to constant weight

(B) Heated at 572*^. to constant weightAmmonium sulphate method100 per cent, sulphuric acid prepared from acid slightly

under 100 per cent100 per cent, sulphuric acid prepared from acid slightlyover 100 per cent

Sulphuric anhydrideSulphanilicacid

97.3397.3597.4197.4297.4197.4197.3997.41

97.4097.4097.4397.41

97.34

97.415

97.41

97.40

97.40

97.415

97.41

The close agreement between the above standards, with oneexception, is only what the writer and his assistants ex-ected,

provided the standards themselves were pure. Theanalyticalmethods employed and to be described yieldresults inexperienced hands that are entirelyin accordance with the abovefigures.

The abnormal result in the case of sodium carbonate ignitedat a low red heat was investigatedas follows:

About 20 grams of sodium carbonate were heated to constantweight at 572'^F.,nd 10 grams used for analysisof the standardacid showed it to contain 97.416 per cent, sulphuricacid. Ten


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ANALYSIS OF. STANDARDS 37

grams were placed in a platinum boat in a combustion tube,whereitwas heated to moderate red heat in a combustion furnace. Aslow stream of dry air,free from carbon dioxide,was aspiratedthroughthe tube, and the carbon dioxide,disengagedby heatingthe sodium carbonate, was absorbed in a satiu-ated solution ofbarium hydroxide,contained in a bottle. A Mohr bulb contain-ng

barium hydroxide was connected with .thebottle and provedthe complete absorption of carbon dioxide therein. After aspi-ating

for several hours, the bulb was connected directlyto thetube and the aspirationcontinued, which showed that no morecarbon dioxide was evolved, no precipitatebeing formed.The excess of barium hydroxide was neutralized with strong

HCl,and finallycarefullytitrated with N/300 hydrochloricacid,usingphenolphthalein as indicator;the barium carbonate wasthen titrated with N/300 hydrochloricacid,using methyl orangeas indicator.A blank titration was made using the same reagents, and the

differencebetween the two methyl orange titrations representedthe alkalinity due to barium carbonate. In this way 0.0060gram carbon dioxide were determined by a titration of aboutJ5 c.c. of hydrochloricacid,thus making a simple and accuratedetermination.^ The carbonate of soda that had been heatedinthe combustion tube was removed, accurately weighed, andDsed to analyze the standard acid. About 10 grams were used,tod the result obtained was 97.358 per cent.,which is 0.058 perBent,lower than the result obtained above.0.0060 gram of carbon dioxide formed by decomposition of

wdium carbonate would leave 0.0084 gram Na20, which, whenweighedand calculated as Na2C03, would make a diflferenceinkheper cent, of sulphuric acid of 0.056 per cent.,which agreeswithin 0.002 per cent, with the result found.

* This method was subsequently published in the Analystj May, 1904,vol.29,pp. 152-153, Thos. Macara.


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After heating to redness:9.9916 grama NasCX)s are equivalent to0.0084 gram NasOOs are equivalentto

9.2369 grains HsS040.0134 gram HsS049.2503 grams SsS04

Before heating to redness:10

.0000 grams NasCX)s are equivalent to 9 . 2447 grams II2SO4

Increased alkalinitydue to Na^O formed 0.0056 gram HSSO4Equivalent to 0.056 per cent, o

H,SO

If the COs found had been the result of decomposition oJsodium bicarbonate,the increased alkaUnitywould have beei0.078 per cent, instead of 0.058 per cent, as found.

By heat:2NaHC0, = NajCOa + CO, + H,0. '

168.116 106.1 44 18.0160

.0060 gram COt found are equivalentto 0 . 0228 gram NaHCOs,After heating to redness :

10.0 grams Na^COs are equivalentto 9 . 2447 grams HsS04

Before heating to redness : 9

.9772 grams NajCO, are 'equivalent to 9 . 2236 grams

0.0228 gram NaHCO, are Iequivalent to 0 . 0133 gram

9 2369 grams 9.2369 grams HSSO4Increased alkalinitydue to formation 0. 0078 gram H2SO4or of NaiCOa from NaHCOj equivalentto 0.078 per cent, of HaS04

iIt is thus indicated by this experiment that the carbori

dioxide formed is the result of decompositionof Na^COa intjNa,0+CO,.


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ANALYSIS OF STANDARDS 39

A sampleof sodium carbonate,prepared by dryingto constantweightat 572**F.,as heated until it had completelyfused,andanalysishowed an increased alkalinityquivalent to 0.30 percent,of carbon dioxide disengaged.Ifthe calcium and magnesium carbonates present in the puri-ied

carbonate were entirelyconverted into oxides when ignitedat low red heat only0.018 per cent, increased alkalinityould beaccounted for.I These results,considered togetherwith the close agreementbetween the other standards and sodium carbonate ignitedat572 F.,re very convincing arguments in favor of preparingifitandardodium carbonate in this manner.

Standard Acid. Âveraging the results obtained from thedifferentstandards enumerated above, exceptingsodium carbon-te

ignitedto redness,its percentage compositionwas found to be97.41per cent, sulphuricacid.This acid or its equivalent was used for standardizingthecausticsoda that was employed for all analyticaldeterminationsembraced in these tables.The burette used was a 100-c.c. chamber burette graduated

from 95-100 c.c. in Jô c.c, and readable to Jôo c c. Theburettewas standardized between 95 and 100 by weighingmer-ury

delivered every }4 c.c, and for 1 c.c. the mercury wasweighed every Jô c.c; the readingsand graduationswere foundto be accurate to }ioo c.c The burette was frequentlycleanedwith strong sulphuricacid,so that it drained perfectlyor eachdetermination.; Standard Sodium Hydroxide Solution. This solution was pre-ared

from cp. caustic soda,purifiedby baryta, and was madeofsuch strengththat 6 grams of standard acid required95-98 c.c.Causticsoda purifiedby alcohol is not suitable for this piupose,as itdoes not drain properlyin the burette,but produces an oilyappearance. To standardize this solution,using methyl orange^ indicator,bout 6 grams of the standard acid were quicklyand accuratelyweighed out, diluted with about 400 c.c cold dis-


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tilled water and 1 c.c. of a Ko P^r cent, solution of methylorangeadded. The caustic soda solution was then run in from the 100-c.c. chamber burette until a few tenths of a cubic centimeter ex-ess

had been added, and after 3-min. drainingthe burette wasread. Standard sulphuricacid of strengthabout equivalentothe soda solution was added from a burette until a trace changedthe color of the solution from yellowto orange. The end pointis sharperin titratingrom alkaline to acid than vice versa,H2SO4 taken H2SO4 2d titration i? 1 1 -j

^ p^-pj = grams of sulphuric acidc.c. i N aw Xxequivalentto 1 c.c. sodium hydroxide solution.

A thermometer was kept in the standard solution,and thetemperature at which the solution was standardized was re-orded,

and in making a subsequent titration at any other tem-eraturethe necessary correction was applied to the reading.

The correction for temperature was determined with the pic-nometer, as described above, and for 100 c.c. of solution wasfound to be 0.015 c.c. = 1**F.,o be subtracted when the tem-erature

was above the temperature of standardizing,and addedwhen below.

Duplicate titrations agreed within 0.03 c.c. Methyl orangewas used in titrating nitric acid, hydrochloric acid andammonia. i

To standardize with phenolphthalein,bout 6 grams of thdstandard acid were accuratelyweighed out and poured into acasserole containingabout 25 c.c. of cold water, all acid bein^rinsed from a small weighing beaker into the casserole. Ondcubic centimeter of phenolphthaleinsolution (1 gram p)er liter)was added, and the sodium hydroxide solution run in from thfl100-c.c. chamber burette until within about 0.5 c.c. of the encpoint. The solution was then boiled for 5 min. to remove carboijdioxide,nd the titration finished by cuttingthe drops from th^tipof the burette until a fraction of a drop produced a faint pincolor. This tint was carefullyoted,and allanalysesrun to tb


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NITRIC-ACID TABLE 41

same end point. By boilingfor exactly5 min., provisionwasmade for uniform drainingof the burette. Duplicate titrationsagreed within 0.02 c.c.While the limits of burette reading were placed at 0.03 c.c.when methyl orange was used,and 0.02 c.c. for phenolphthalein,yet, as will be shown, the actual duplicatesobtained by two menworking independentlyaveraged much closer.Dividing Burette. The dividing burette referred to under

standardizingwith sulphuricanhydride is designedfor accuratelydividinga solution. It consists of a burette the top of which isdrawn to a capillarynd bent downward; the stop-cockof theburette is a three-way cock, the third passage being connectedto a vertical tube at the top of which is a funnel forfillinghe burette. One and 2-liter flasks with small neckswere graduated by running from the burette a sufficient numberof times to fillthe flask to a point in the neck. This point wascarefullychecked,and in subsequent use, it was always filledto this mark.

The amount of water deUvered by the burette was weighed,and the weights checked within 0.004 gram, or J^5,ooooi theweight of one burette full. In measuring out an equivalentof5 grams of a liquidmade up to volume, the error would be 0.0002gram.The tables are described in the order in which they were pre-ared

during a periodof nearly3 years.

NITRIC-ACm TABLE

The c.p. nitricacid employed was free from nitrous and hydro-hloricacids,and the residue upon evaporation at 212 F. wastoo small to aflfectthe determinations. This acid was used forallsamples up to 43 B6.,and for the stronger samples this acidwas concentrated by distillingith pure glacialphosphoricacidand potassium permanganate, the latter to prevent the formation


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of nitrous acid. 95.80 per cent, nitric acid was the strongestsample obtainable, for above this point the acid contained largeamounts of nitrous acid.

The specific-gravitydeterminations were made as describedabove, and at the same time the picnometer was filled^ 6 to8-gram sample was weighed in a small weighing tube having aground-glass stopper, which prevented loss while weighing anddiluting. The sample was diluted with water by removing thestopper of the tube with a glassfork while immersed in a casserolecontaining approximately 400 c.c. of water. The titration wasthen made, using methyl orange as indicator,observing the con-itions

described in standardizing.Allowance for Temperature. After determining the specific

gravity of the different strengths employed at 60 F., the tem-eraturewas raised to 70 F., and the picnometer weighed; like-ise

at 80 F. from this data the allowance for temperaturewas calculated,and was found to be uniform for a givenstrength of acid. At 43 B6. the determinations were madefrom 50 to 90 *?.

The following determinations were made, and from these thetable was calculated by interpolation,the specificgravity andcorresponding percentage composition being calculated to cor-espond

with each 0.25 B6.From the Baum^ the corresponding specificgravity was calcu-ated

by the formula:

Degrees Baum^ = 145 Specificgravity

The instabilityf 96 per cent, nitric acid is so great that agree-ngdeterminations were difficult to obtain, and those selected

corresponded with the differential of the table at this point.


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HYDROCHLORIC-ACm TABLE

The purest c.p. hydrochloricacid obtainable was tested foifree chlorine,sulphuric acid and residue upon evaporation atl212 F. There were only traces of impurities,hich would aflfecthe determinations less than the errors of manipulation.

For the samples above 22 B^. this acid was concentrated bydistillingt into a portion cooled in ice water. 42.61 per cent.ihydrochloricacid was the strongestsample upon which a specific-gravity determination could be obtained at 60 P. Above thispointbubbles of gas were formed in the picnometer when warmedto 60^F.

The specificgravity and allowance for temperature weredetermined as in the case of nitric acid. The allowance for tem-erature

was found to be uniform for each strengthof acid;22**B^. deteminations were made from 50 to 0O F.

After making the above determinations the thermometer ofthe picnometer was withdrawn while the bottle was immersed inabout 700 c.c. of water in a large casserole,hus avoidinglosswhile diluting. The bottle was carefullywashed out and thedilute acid made up to 2 litersin a flask standardized againstthe100 c.c, dividingburette and portionsof this solution wete takenwith the burette for titration with sodium hydroxide. Methylorange was used as indicator,he same conditions used in stand-rdizing

being closelyfollowed,about 98 c.c. of sodium hydroxidesolution being used for each determination. A sample of hydro-hloric

acid was analyzed by precipitatingith silver nitrate andthe silver chloride calculated to hydrochloricacid checked theresults obtained by titration.


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HYDROCHLORIC-ACID TABLE 45

The followingdeterminations were made, and from these thetable was calculated by interpolation,he specificgravity andoorrespondingercentage composition being calculated for each1^. from 1^-5^, 0.25^B6.,rom 5^-16'' and for the rest of thetablefor each 0.1 B^.

The following will show the comparative sensitiveness of theanalyticaldeterminations, specificgravity determination andreadingf a delicate Baum^ hydrometer and thermometer gradu-ted

to l^F. in terms of specificgravity:


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SULPHURIC-ACID TABLE

The c.p. sulphuricacid used was 1.84 specificravity,Tiraifree from hydrochloricand nitric acids and ammonia and gave itrace of residue upon evaporation. The impurities were leathan enough to affect either the specificgravity or analjrticadeterminations.

The specific-gravityeterminations were made as describeeabove, except that in bringing the temperature to 60 F., thpicnometer was immersed to the neck in a beaker of water a fe^degrees below 60 F.,so that the temperature rose slowly,bein|the same inside and outside when capped.

The allowance for temperature for every 10**P. between 50^and 90^F. was determined at the following degrees Baum^66, 63, 57, 51, 44, 36, 29, 21, 12. It was found to be practicalljuniform for a given strengthof acid,and the results are based ora range of 40 F.,the table givingthe corrections at even degreesBaum^, being calculated from these results by interpolation^Samples were taken from the picnometer for analysis,nd aEamount of acid was weighed out each time which would requirebetween 95 and 100 c.c. of soda solution. With the weakestsamples a more dilute standard soda solution was used, but thesame conditions as used in standardizingwith phenolphthaleinwere closelyobserved in all cases.

The boiling-pointeterminations were made in a 200 c.c. long-necked flask,using about 100 c.c. of acid in each case. A certi-ied

thermometer accurate to 1 F. was suspended in the acid.A small pieceof porcelainwas placed in the bottom of the flaskto facilitateboiling. The flask was graduallyheated with a freeflame and the temperature recorded when boilingwas firstperceptible.

The followingdeterminations were made, and from these thetable was calculated by interpolation,he specificravityand thecorrespondingpercentage composition being calculated for eachdegreeBaum6 from 0 -64 and for each }i'*B6.rom 64^- 6''B^,


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SULPHURIC-ACID TABLE 47

From the Bailing the correspondingspecificravitywas calcu- 145latedby the formula: Degrees Baum^ = 145 ^ r- .^ ^ specificgravity

The degree Twaddle was calculated by dividingthe decimalpartof the specificgravityby 0.005.


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The followirig will show the comparative sensitiveness of theanalytical determinations, the specific-gravity determinations,and the reading of a delicate Baum^ hydrometer and thermometergraduated to l^F., in terms of a specific gravity:

The following chemists, my assistants,* aided in the preparationof the tables :

W. P. Kern, B. S.J. G. Melendy, B. S.Hardee Chambliss, M. S., Ph. D.H. B. Bishop, B. S.W. W. Sanders, B. S.

T. Lynton Briggs,

N. A. Laury, B. S.A. J. LOTKA, B. Sc.C. A. BiGELow, B. S.A. F. Way, B. S.

'

H. P. Merriam, Ph. D.F. I. C, F. C S.

Such merit as these tables possess is largely due to these gentle-en,but more especially to Mr. Bishop who had immediate

charge of, and participated in most of the determinations, andwho shared with the writer the preparation of this paper.


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NITRIC ACID 49

Nitric AcidBy W. C. Ferguson


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50 SULPHURIC ACID HANDBOOKNitric Acid {Conduded)

Specificgravity eterminations were made at 60**F.,compared with water at 60^F.Prom the specificgravities,the corresponding degrees Baum6 were calculated by tlfollowingformula: -^ , ^ -.ab^ 145Degrees Baume = 145 r= rrspecificgravityBaum6 hydrometers for use with this table must be graduated by the above formulwhich formula should always be printed on the scale.Atomic weights from F. W. Clarke's table of 1901. O - 16.

Allowance for TemperatitrbAt 100-20* B6. Ho^B^. or .00029 specificgravity - VF.20* -30* B6. V^8*B6. or .00044 specificgravity - 1*F.

30' -40* B6. V^o*B6. or . 00060 specificgravity - 1*F.40' -48.5 B6. H7 B6. or .00084 specificgravity - 1* F.Authority W. C. FergusonThis table has been approved and adopted as a Standard by the Manufacturing Chemisi

Association of the United States. W. H. Bower, Jab. L. Morgan,Hbnrt Howard, Arthur Wtman.A. G. ROSBNGARTEN,few York, May 14,1903. Executive Committee,


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Specific-gravityeterminations were made at 60 F.,compared with waterat 60 F.

From the specificravities,he correspondingdegreesBaum4 were calcu-ated by the followingformula:

Degrees Baum4 = 145 r^ ^:specificgravityAtomic weightsfrom F. W. Clarke's table of 1901. O = 16.Allowance for Temperature10-15 B6. Ko B^. or .0002 sp. gr. for 1 F.15-22 B6. Mo B^. or .0003 sp. gr. for TF.22-25**B6. M8 B6- or .00035 sp. gr. for l^'F.Authority W. C. Ferguson

This table has been approvedand adopted as a Standard by the Manufac-uringChemists' Association of the United States.W. H. Bower, Jas. L. Morgan,Henry Howard, Arthur Wyman.a. g. eosengarten,

V York, May 14,1903. Executive Committee.


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TABLE OF SULPHURIC ACID

By W. C. Ferguson and H. P. Talbot


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54 SULPHURIC ACID HANDBOOKSulphurk; Acid

By W. C. Fbrouson and H. P. Talbot

SpecificGravity determinations were made at 60**F.,ompared with waterat 60*'F.

From the SpecificGravities,the corresponding degrees Baum6 were cal-145culated by the followingformula: Degrees Baum6 = 146 ^ .^ p r

Baumi^ hydrometers for use with this table must be graduated by theabove formula, which formula should always be printed on the scale.

66 B6. = specificgravity 1.8364 = Oil of Vitriol (O. V.).1 cu. ft. water at 60''F. weighs 62.37 lb. av.Atomic weights from F. W. Clarke's table of 1901. O = 16.

H2SO4 = 100 per cent.Percent. Percent Percent.HaSO* O. V. 60

100.00 = 119.9883.35 = 100.0066.72 = 80.06


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SULPHURIC ACID 55

SuLPHXTRic AcidBy W. C. Ferguson and H. P. Talbot

Acids stronger than 66**B6. should have their percentage compositionsdetennined by chemical analysis.

Authorities W. C. Ferguson; H. P. Talbot.This table has been approved and adopted as a standard by the Manu-acturing

Chemists' Association of the United States.W. H. Bower,Henry Howard,J AS. L. Morgan,Arthur Wyman,A. G. Rosengarten,

New York, June 23, 1904. Executive Committee,^ Calculated from Pickering'sresults,our, Lon, Chem. Soc.,vol. 67,p. 363.


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56 SILPHCRIC ACID HANDBOOK

Sn^pHTRic Acid (Continued)


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SULPHURIC ACID 57

SuLPHUBic Acid {Continued)

^culatedfrom Pickering'sresults,Jour. Urn, Chem, Soc.,vol. 57, p. 363.


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Sulphuric Acid (Concluded)


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SULPHURIC ACID94r-100 per cent. H2S04^

H. B. Bishop

The acid used in this table was preparedfrom c.p. 95 per centsidphuricacid,which was strengthenedto 100 per cent, by thaddition of fuming acid made by distillinguming sulphuric ac(70 per cent, free SO3) into a portion of 95 per cent. c.p. acidThe final acid was tested for impurities;residue upon evaporation,chlorine,niter and sidphur dioxide (0.001per cent.)'whiclwas less than the sensitiveness of the determination.

The analyticaland specific-gravityeterminations,and thiallowance for temperature were made in the same manner, an^with the same accuracy as in the sulphuric-acidtable adopteby the Manufacturing Chemists' Association,he specificravit]1.8354 and 93.19 per cent. H2SO4 being taken as standard.

The actual determinations were made within a few hundredth^of a per cent, of the pointsgiven in the table,the even percentagebeingcalculated by interpolation.

1 W. W. Scott: Standard Methods of Chemical Analysis, 1917.


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SULPHURIC ACID 61

Authob'b Note. Mr. Ferguson in his articledescribinghe methods usedin the preparation of the tables adopted by the Manufacturing Chemists'Association names several chemists who assisted him, among them Mr.Bishop. Such merit as these tables possess is largelydue to these gentle-en,

but more especiallyto Mr. Bishpp who had immediate charge of andparticipatedin most of the determinations,nd who shared with the writerthe preparation of this paper.

SULPHURIC ACID0**B6.-100 per cent. H2SO4

f From 0 -66*^B6. the table is from the one of Ferguson andPTalbotwith the followingsupplemental incorporated:

Per cent. SO3Pounds SO3 per cubic footPounds H2SO4 per cubic foot

I Per cent, free waterI Per cent, combined waterFreezing (melting)pointscalculated in degreesCentigradefrom

Ithegiven degrees Fahrenheit.I Approximate boilingpoints calculated in degrees Centigradefrom the given degreesFahrenheit.

Allowance for temperature calculated per degree Centigradefrom the given,per degreeFahrenheit.From 94-100 per cent. H2SO4 is from the table of H. B. Bishop.

Mr. Bishop gives only the specificgravity and allowance fortemperature per degreeFahrenheit. All other calculations aresupplied.Freezing (melting)pointswere calculated after Knietsch,Ber.,1901.It should be noted that the highest percentages show lower

specificgravitieshan those just below, the maximum being at97.5 per cent. H2SO4.


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62 SULPHURIC ACID HANDBOOKSulphuric Acid

0**B6.-100 per cent. HjSO*


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SULPHURIC ACID 63

Sulphuric Acid0*B^.-100 per cent. HjSO*


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Sulphuric Acid0 B6.-100 per cent. H2SO 4 (Con^int^ed)


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SULPHURIC ACID 65

SuLPHXTBic Acid0**B^.-100 per cent. H,SO 4 (Con/int*cd)

DesreeeBaam4

Per cent.H S04

4041424344454647484950515253545556575859606162636464M64H645i6565K65^66

Per cent,freeH,0

Per cent,combin dHsOe

Per cent.O. V.

Lb. O. V.in 1 cu. ft.

Freesing (melting) points

F.

94.0095.0096.0097.0097.5098.0099.00

100.00

51.9050.5349.1347.7446.3444.9343.5242.1040.6839.2537.8236.3434.8733.3731.8730.3528.8327.2525.6424.0122.3320.5718.7016.6614.3413.6712.9612.1911.3510.459.408.206.816.005.004.003.002.502.001.000.00

8.839.099.349.609.86

10.1110.3710.6310.8911.1611.4211.6911.9612.2412.5112.7913.0713.3613.6613.9614.2714.5914.9315.3115.7415.8615.9916.1316.2816.4516.6416.8617.1217.2617.

sulphuric acid handbook 1000265717 (1)

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