PAPER; GENERAL SPECHUCATIONS AND METHODS OF ~ESTINGeveryspec.com/FED_SPECS/U/download.php?spec=UU-P-31B.032687… · uu–p–31b 3 march 1949 federal paper; general superseding fed

UU–P–31b3 MARCH 1949

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FEDERAL

PAPER; GENERAL

SUPERSEDINGFed. Spec. UU.P-31.June 17, 1937

SPECIFICATION

SPECHUCATIONS ANDMETHODS OF ~ESTING

Thi# 8peci@twn ww approved bu the Commi88wner, Federa3 SUPPIUService,General Servue8 Admintitw tion, for the NW of all Federal (,.gewim,

1. PUBPOSE AND SCOPE

1.1 This specification covers the generalrequirements and methods of testing that arecommon to paper, paperboard, and convertedpaper products covered by Federal specifica-tions. This specification does not include testmethods applicable only to a specific.product;such test methods are included in the detailspecifications. In the case of conflict betweenthe provisions of this specification and thosdof the detail specification for a particularmaterial or product, the provisiona of thelatter shall take precedence.

1.2 The detail specifications for the vari-ous types of material represent the lowestquality that will be accepted. All detail speci-fications definitely state the minimum ormaximum limit as to stock, strength, foldingendurance, or other qualitiea which will beaccepted. Contractors shall adjust their ma-terials and processes so as to insure the de-livery of finished paper which will fully com-ply with the requirements of the specifica-tions.

2. GENERAL BEQUIRE$fENTS

2.1 Curl.—Paper having a curl whichcannot be overcome under reasonable work-ing conditions may be rejected.

2.2 Size and trim.—Paper shall bc full

size when delivered. Coated book, writing,map, chart, lithograph, manifold, bond,parchment, ledger, and index paper shall betrimmed square on four sides. Other flatpaper shall be cut square on four sides. Atolerance of one-sixteenth inch in size willbe allowed, unless otherwise specified.

2.3 Count.-’’Mill count,” 500 perfectsheets to the ream, shall be accurate for allgrades of paper. Verification of “mill count”will be made by the receiving office and de-liveries may be rejected for incorrect count.Shortage will be deducted in case the deliv-ery is accepted.

2.4 Roll winding.-Roll paper shall betightly wound, at even teneion, and shall con-tain the least possible number of splices.Splices shall be neatly made and be flaggedat both ends of the roll with projecting col-ored markers. Any roll shall not containmore than four splices.

2.5 Bcais weight tolerance. — Un Iesaotherwise specified, any variation above orbelow the basis weight specified shall not ex-ceed 5 percent.

2.6 Thickness tolerance.—Where an av-erage thickness is specified, the followingplus or mirius tolerances will be allowed: upto .012 inch, tolerance .0005 inch; .012 ti

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UU-P-3 lb

.016 inch, tolerance .0008; above .016 inch,tolerance .001 inch.

2.7 Watermark.-Paper furnished underthe specifications for 25-, 50-, and 100-per-cent bond, and ledger papers shall be water-marked with the seal of the United States,together with the symbol designating thegrades, as provided in the detail specifica-tions. The watermark shall be clear andlegi~ , and shallappear on a basis of fourtimes on sheets 16 by 21 inches, once in eachquarter. Copies of full-size watermark de-sign for each of these types of papers will hesupplied upon request by the Public Printer,Government Printing Office, Washington 25,D. c.

2.7.1 Contractors will be permitted tosell mill sortings and rejected stock bearingthe Government watermark. The Govern-ment watermark shall not be applied to anypaper other than that ordered by a dulyauthorized officer of tbe United States Gov-ernment.

2.8 Definitions.

2.8.1 Tub-sized.—The term “tub-sized”in detail specifications shall be construed tomean that the paper has been passed througha bath of sizing material.

2.8.2 Ruling, writing, and erming qua2Lties.—Where the requirement “shall be suit-able for ruling and writing on with ink, andshall have good erasing quality” appears ina detail specification, it shall be corrgtrued tomean that lines ruled or cbaractere writtenwith ink shall be clear cut; and that aftererasure of ruled lines and written or typedcharacter, the paper shall have retention ofgood writing and typing quality, and appear-ance of surface.

2.9 Sampling and inspection.

2.9.1 Unless otherwise specified, pur-chasesshall be inspected and samples for teettaken at the point of delivery. If the inspec-tion and tests, whether preliminary or final,are to be made on the premizes ot’ the con-tractor or subcontractor, the contractor shall

furnish, without additional charge, all rea.sonable facilities and assistance for the safeand convenient performance of the inspec-tions and tests. The manufacturer andior ●the contractor shall notify the purchasingofficer sufficiently h advance of the comple-tion of manufacture of material to permitarrangement for inspection and selection ofsamples.

2.9.2 The number of samplee ~ be se-lected from each lot shall be as specified inthe detail specification. The num&r of Speci.mens to be tested in each type of test shallbe as specified in thedetaiI specification; ifnot so specified, at least five specimens shallbe teeted.

2.10 Remrlts of tem~.

2.10.1 Unless otherwise specified, theaverage of the resulte for the specimenstested shall be ueed to determine conform-ance of materials tested under this specifica-tion.

>2.10.2 Unless otherwise specified, results

that deviate from the mean value of all teetashall be rejected if tbe deviation of thedoubtful value is more than five timee theaverage deviation from the mean obtained by ●excluding the doubtful value. Additionalspecimens ehall be teeted in place of any forwhich the results are diecarded in accordancewith these provisiona.

2.11 Latent defect.e.-If latent defectsshould be discovered after material has beenaccepted, the contractor shall, if required,replace the defective material without costto the Government.

3. NOTES

3.1 Paymant baaM.-Roll paper will bepaid for at gross weight, exclusive of return-able coreg, unless more than 2% percent overthe ordered basis weight, in which case theweight in excess of 2% percent will he de-ducted. Flat paper will be paid for at theordered basis weight to the nearest 2%pounde, unless more than 6 percent underweight, in which caee payment will be made

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UU-P-31b

for actual scale weight, including wrappersand twine.

3.2 Additional details of testing methods.—For further details of testing methode de-scribed herein, the methods of the TechnicalAssociation of the Pulp and Paper Induetry(T.A.P.P.I.) listed should he consulted.These may be obtained from the Associationat 122 E. 42nd Street, New York 17, N. Y.

25,D.C.(mlda .X91.Sd thismdllcdl. d Ocmr Prtit SFadfi.tl’aa

ri.wli-edb?SCtlrklescmmcb W Feral hemmed forMdnw Fur-Wma UOanuable Witbutciur@u timae.ml %m.* Adrdi*str8-tb R@d MI..& East-. W York,Atla!$%ChIuK’J,KarQ.uml, u.. , mu-, mm-’, h Fn.lc-co,J-mAQgebc.,a.ulm,amW—, D.C.(r&ml C2Lwernm.tutilitiesrc.s,Cbtuncm., ‘dF*ml ETQdu-

Cau. andmmdu&d lb W.d F&ml mdfldlcmsandmand-8F3S*cmestablisheddiatriLam.Lwimtminml, agmcles.)

Patentm.tice.-WhenGovernmentdrawings,speci-fications,or otherdata are used for any purposeotherthan in connectionwith a definitelyrelatedGovernment procurement operation, the UnitedStatesGovernment therebyincursno responsibilitynor any obligatim whatsoever; rmd the fact thatthe Government may have formulated,furnisl@ orin any way supplied’the said drawings pecifica.

#tions,or other data,isnot to be regar d by lmpl,-catim or otherwiseas in a“y me.n,tirlicensingtheholderor any other person cm cerparatio”,or con-veying any rightsor permiss~on to manufacture,use,or sellany patentedinventionthatmay in anyway be relatedthereto.

4. NAVY ACTIVITIES INTERESTED

MCMOShSY

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uU-P-3 lb.3MARCH 1949

INDEX OF TEST METHODS

PHYSICAL TESTS

MethodNo.

Adhes~on of Pressure-Sensitive Tapes .................................................100

Adhesion of Scale and Closures for Packages ... .................................101

Atrnosphe,r]cCondlt]ons .........................................................................102

BasM Weight ...........................................................................................110

Brigh~ness ..............................................................................................111

Bur~tlng Strength ........................................... ...................................- -- 112

creasing for Water and Water-Vapor Resmtance Tests ..................120

Finish (Smoothness) ............................................................................130

Folding Endurance, Schopper ..............................................................131

Folding Endurance, M.I..T.....................................................................132

Machine DirectIon (Gram) .................................................................140

Oil Penetration ................................................................................... . 150

151opac,~y .......................................................1..............................- . . ... .

Samphng and Preparation of Test Samp e .......................................160

Tearing Reelstance ....--...-..-----..---..-.-.---.---..-""-"-"".--"-""---"""---""--"""--" ““”170

Tensile Breaki,ng Stren@h (DIY) and Elongation.. -----”---”--””--””-““’171

Tensile Breaking Strength, Wet ........................................................172

Thickness ................................................................................................- 173

Water Ahs$@lVeness ---...-.---..-...-.--.---..---..--"""---"--"""----"""---"---""--"- ‘“””180

Water Resistance ........ .. ..................................................................... 181

water vap~~ permeability ..................................................................182

Wire and Felt Sides.............................................................................. 183

CHEMICAL TESTS

I .An

Acidity, pH ----..-......--..-.....-.----..--.---"""---"--"`"""""""`""""""`""""""""""`"""`Alpha Cellulose ...................................................................

..................... 201

Aah ............................................................................................................ 202

Copper Number ...................................................................................... 220

Momture ....................................................................................................240

Rosin ....................................................................................................... 250

Fj~r ldentifi~tiOn and Quantitative Determination. ..............-..--------300

,A.P,P.INo.

T806smT402mT410mT452mT403m

T423mT423mT409mT462mT425mT400mT414mT404mT456mT411mT432mT433mT448mT455sm

T435mT429mT413mT430mT412mT408m

I T401nr

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Method 1003 MARCH 1949

● ADHESION OF PRESSURE-SENSITIVE TAPES

1. Scope

1.1 This method is intended for testingthe adhesion of pressure-sensitive papertapes and cellulose tapes.

2. Test specimen

2.1 The test specimen shall he about 203millimeters (8 inches) long and not morethan 25.4 millimeters (1 inch) wide.

3. Apparatus

3.1 A pendulum-type tensile testing ma-chine as described in method 171.

3.2 A 5“ x 2“ x +.” stainless-steel platepolished to a No. 4 finish (commercial polishground ) as specified in Federal Specification

1QQ-S-766.

3.3 A 4Y&pound rubber-covered rollerapproximately 31/2inches in diameter by ls~inches in width, the surface of which has adurometer hardness value within the range

●70-80.

4. Prncedure

4.1 Before each test, wash the polishedsurface of the steel plate thoroughly withcarbon tetrachloride, using a clean piece oflintless wiping tissue for each washing.After all tracee of the carbon tetrachloridehave evaporated, wipe the surface of theplate with a clean dry piece of the tissue.Apply the tape, adhesive side down, to the

polished surface of the plate with a 5-inchsection extending beyond one end of it. Pressthe tape down firmly by passing the rollertWiCeover its surface in opposite directionsat the rate of approximately 12 inches perminute, using the weight of the roller only.(Pumice, French talc, or a strip of papermay be applied tu the adhesive side of theextended section of the tape to prevent ad-hesion during the rolling. ) Immediately dou-ble-back the free end of the tape at an angleof 180” and peel 1 inch of the tape off theplate at the folded end. Clamp the adjacentend of the plate into the lower jaw of thependulum-type tensile machine and the freeend of the tape in the upper jaw. The pawlson the pendulum arm shall be taped back inan open position. The tensile tester shall beof such capacity that the test values will beread when the pendulum hangs between 9°and 45° from the vertical. After the firstinch is removed from the plate during thetest, the minimum tension required to re-move the remainder of the tape, except forthe final 1 inch, from the plate shall be takenas the adhesion value. The test shall be madewith the stressing jaw moving at a speed of12 inches per minute.

5. Report

5.1 The average adhesion value for notless than five specimens shall be reported inounces per inch width to one decimal place.

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Method {013 MARCH 1949

ADHESION OF SEALS AND CLOSURES FOR PACKAGES ●1. scope j usting the length, whenever possible, so that

1.1 This method is applicable for testingthe material extends about 1IA inches beyond

the adhesive used in forming seals, closures,the cemented joint.

and seams of heavy paper or paperboard 3. Procedurepackages, It indicates the suitability of tbeadhesive for the specific material on which it

3.1 Grasp each projecting end of the

is to be used.specimen between tbe thumb and forefingerof each hand, the forefingers resting against

2. Test specimens the cemented joint, one on each side. Sepa-

2.1 If finished seals are not available,rate tbe joint by gently pulling the ends

prepare a seal with the adhesive and withapart with a rolling motion from the top

the materialon whichtheadhesiveistobe downward withthesecondjointsofthesec-

used. Condition two pieces of the material,ond and third fingers successively resting

against each other to act as fulcrums. Esti-each 12 by 31/2 inches, and cement them to-

gether with the adhesive with a joint 2mate the percentage of separation of the

inches wide along the 12-inch sides, applyingjoint that occurs without fiber separation

the adhesive as in actual use. Allow to con-from the surface of the paper or paperboard.

ditionfor 24 hours,then cut across the joint 4. Reportintostrips1 inch wide.

4.1 The average percentage of separa-2.2 If finished seals or seams are avail- tion without fiber failure, of the joints of not

able, cut strips l-inch wide across them, ad- less than 10 strips shall be reported.

.,

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●ATMOSPHERIC CONDITIONS

Method 1023 MARCH1949

1. Hurrridityand temperature

1.1 Unless otherwise specified in the de-tail specification, all physical tests of paperand paper products shall be made on sam-plas conditioned in an atmosphere main-tained at 60 & 2 percent relative humidityand 23° & 2“C. (73° & 3.5”F.), and thetests shall bs made under these atmosphericconditions.

2. Conditioning

2.1 Suspend each test specimen of thesample so that the conditioning atmospherewill have free access to all surfaces. Maansshall be provided for so circulating the airof the conditioning and testing chamber that

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its humidity and temperature will he uni-formly maintained throughout the chamber.The conditioning time shall be sufficient forthe moistnre content of the specimens to at-tahr equilibrium with the conditioning at-mosphere. Determine this by conditioning

●until there is no significant change in theweight of the specimens (i.e. less than 1 partin 1,000). For papers that are not highly r-sistant to water vapor, weigh at intervals ofnot less than 2 hours; for highly resistant

papers such as hard, surface-si=f bOnd andledger papers, at intervals of not less than12 hours; for papers that have been givenspecial treatment for resistance of watervapor, and for paperboards, at intervals ofnot less than 24 hours.

3. Determination of humidity and temper.ml-c

3.1 Determine the relative humidity ofthe conditioning atmosphere by means ofeither (1) a sling psychrometer, or (2) astationary type of psychrometer having theair circulated over the bulbs of the ther-mometers mechanically. In both cases thecirculation of air around the bulbs shall beat the rate of not less than 3 meters (10 feet)per second and the exposure not less than 60seconds before the readings ire taken. Whenthe sling type is used, make the readings, es-pecially of the wet bulb, as quickly as possi-ble after bringing it to rsst.

3.2 The thermometers used shalI b-e ac-curately calibrated by comparison with cer-tifisd standard thermometers and any cor-rections found necessary applied te the read-ings.

UU-P41b



BASIS WEIGHT

1. Definition

1.1 The basis weight of paper and pa-perboards is the weight in pounds of a givenarea which varies for different kinds.

2. Test specimens

2.1 The specimens of paper for teat shall

~consist, whenever possible, of not less than10 sheets, each at least 100 square inches inarea. The mrecimen of DaDerboard for teat. .shall consist, whenever possible, of not lessthan 5 sheets, each at least 1 square foot inarea.

3. Apparatus

3.1 The balance used shall have a sensi-tivity of not more than 0.25 percent of theload applied and shall be ao graduated thatreatilngs of this degree of accuracy can bemade. Tbe balance shall have been calibrated

not more than 30 daya prior to the teat, bothwith increasing and decreasing loads by ap-plying accurate weights.

4. Procedura

4.1 The area of the specimen shall be de-termined to the nearest 0.25 percent of itstotal area, which requires a precision of 0.1percent in measuring the dimensions. Theweight of the spscimen shall be determinedto the nearest 0.25 percent of its totalweight. Calculate the basis weight from themeasured area of tbe specimen and itsweight.

5. Report

5.1 Report the basis weight of paper inpounds per ream of sheeta of stated numberand size, and the basia weight of paperboardin peunds per 1,000 square feet. The weightshall be reported to three significant figures.

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● BRIGHTNESS

Method 111s MARCH1949

L Definidon

1.1 Brightness is the ratlactance of whiteand nasr-white papers to iiiht in the blueand violet portions of the spectrum. Bright-ness mcaeurements of such papers correlatewell with subjective estimates of their. rels-tive whitenacs.

2. Teat SpdSIWll

2.1 The test epaciman shell consist of apad of sheets of the size suitable for the apparatus used and the number of sheets beingsuch that when arranged in a Dad, the brighhness of it is not cbangcd by doubling itathicknaes. The arcs of the test specimen ueadfor the meaaurament shall be frae from

/1 watarmark and any blemish that might af-fact the mcaeuremcnt.

3. Apperatnn

3.1 The apparatus shall be a reflactioq

●mater of such design and adjustment that itareadings correlate satisfactorily with read-

ings made by the master instrument of theTechnical Association of the Pulp and PaperIndustry.

A Procednrc

4.1 All maasurementa shall be made onthe felt side of the paper. Place the pad ofpaper over the sample aperture of the instru-ment with the machine direction of the papa’parallel to the plane determined by the axcaof the incident and rcflactad rays of light.Place a l-kilogram weight having a planebase upon the pad. Measure and racord thebrightness reading to a 0.1 unit. Move thelower shad of paper to the back of the padand make snother brightnces determination.Repast this procadure until six differentshcats of the iad have been tested.

5. Rapoti

5.1 The report shell state the averagepercentage of brightness (based on magn-esium oxide = 100) to one decimal plccc.

uu-P-31fY


BURSTING

1. Stops

1.1 Thk method is designed to measurethe bursting strsngth of paper and paperproducts having a bursting strength of notover 200 points, and in the form of sheets notover 0.025 inch thick.

2. Test specimens

2.1 The test specimens shall bs at least63.5 by 63.5 millimeters (2.5 by 2.5 inches).

3. Apparatus

3.1 The testing machine shall havemeans for firmly clamping the test specimenwithout slippage during the test, betweentwo annular, plane, unpolished (matte) sur-faces, which may have fine, concentric toolmarks not over 0.002 inch deep. The upperclamping surface (clamping ring) shall havea circular opening 1.200 & 0.001 inches indiameter. The circular edges of the openingswhich are in contact with the speeimen andrubber diaphragm during testing shall berounded off to a radius of not over 1/64 inchto avoid any cutting action. The lower clamp-ing surface (the diaphragm plate) shall be0.125 inch thick and shall have an opening1.25 * 0.01 (1.24 recommended) inches indiameter. The clamping ring shall be con-nected to the clamping mechanism througha swivel joint to insure an even clampingpressure. During the tests the circular edgesof the opsnings in the two clamping platesshsll he substantially concentric, with nooverlapping at any point.

3.2 A rubber diaphragm fres from min-eral loading material and .033 to .035 inchthick, shall be clamped between the lower

Method 1123 MARCH 1949 .

STRENGTH

clamping plate and the rest of the apparatusso thst before the diaphragm is distended bypressure underneath, it, the center of. the up-per surface is below the plane of the clamp-ing surface.

3.3 There shsU be means for applyingcontrolled, increasing hydraulic pressure tothe underaide of the diaphragm until thespecimen bursts. This pressure shall be gen-erated by a piston forcing a liquid (usuallyglycerine) into the pressure chamber of theaPParatus at the rate of 95 & 10 millimetersper minute (motor-driven) or at the rate of120 revolutions per minute (hsnd-driven).

3.4 The apparatus shall be equippedwith a pressure gage of the Bourdon-tubemaximum-reading type graduated in poundsper square inch and accurate throughout theentire range of its scale to within a valueequal to 1.0percent of its maximum capacity.This gage shall be such that the individualreadings will be not less than 25 percent normore than 75 percent of the total capacityof the gage.

4. Procedure

4.1 Clamp the specimen seeurely in posi-tion, apply the hydrostatic pressure as speci-fied in 3.3 until the specimen ruptures, andrecord the maximum registered by the pres-sure gage. An Wual number of tests shallbe made on each side of the paper.

5. Report

5.1 Report the average of the test resultsof not less than 10 spscimena in points (ap-proximately pounds per square inch) to thrsesignificant figures.

2.

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CREASING FOR WATER AND WATER-VAPORRESISTANCE TESTS

1. Scope

1.1 This method is to provids reproduci-bly creased specimens for teata of papers andother thin sheet materials used for packag-ing.

2. Teat .specimena

2.1 Whenever possible, the test specimenshall be 76 by 76 millimeters (3 by 3 inches).

3. Apparatus

3.1 The apparatus shall consist of asmooth, flat base plate having hinged to itat one edge a top plate capable of matchingand surfacing the base plate, and weighing

10 pounds.

4. PrOcedurs

Al Fold the test specimen without creae-ing it eo that corners of the sheet diagonallyopPosite coincide. Place the folded specimenon the base plate of the apparatus with thefold towards the hinge. Position the topplate so that its center is directly above thefold, lower it on tbe specimen, and allow itto remain on the specimen for 30 seconds.At the end of this period, remove the speci-men and repeat the procedure to make acrease on the other side of the specimen, andat right angles to the first crease.

IJU-P-31b



FINISH (SMOOTHNESS)

1. Scope

L 1 This method is for measurement ofthe finish of printing papers with referenceto the printing smoothness of their surfaces.

2. Test sp&imena

2.1 The test c.pecimens shall be 51 by 51millimeters (2 by 2 inches), and shall beclean and free from watermark and fromblemishes that might aff~t the test ~esu]t,such as creases and wrinkles.

3. Apparatus

3.1 The apparatus shall be a Bekksmoothness tester conforming to the follow-ing:

3.1.1 A circular plane surface having aneffective area of approximately 10 squarecentimeters, and a small circular aperture inthe center.

3.1.2 A means of applying a direct pres-sure of 1 kilogram per square centimeter tothis area and a vacuum of 380 millimeters ofmercury.

3.1.3 A means of paasing a known vol-ume of air, 10 milliliters, controlled by thesize of the air chamber, between the papersurface and the plane surface.

3.1.4 A means of measuring the volumeand rate of change in vacuum from 38o mil-limeters to 360 millimeters in paasing theair between the two surfaces.

3.2 The apparatus shall he tested fre-quently for leakage, and the capillary tubaand the pad of the apparatus shall he keptclean.

4. Procedure

A 1 Set the stopcock of the tester to posi.tion “p” with gentle strokes of the vacuum

pump, pull the mercury column slightlyabove 380 and turn the stopcock to position“o”. Place the side of the specimen to betested on the polished glass disc, then lay thesquare of soft gum rubber on the paper andon top of this, center the metal pressure diet.Bring the lever down to a horizontal paitionso that the leveling screw rests on the borein the center of the metal disc. With the aidof the spirit level, and by means of the level-ing screw, maintain the pressure bar in alevel position throughout the test. Turn thestopcock counter-clockwise to position “M”and with the fine regulating vent at the baseof the air chamber, hy a gentle pulling-turn-ing motion, permit the mercury column todrop to approximately 380. Just before themercury column reaches 380, close the fineadjustment vent with a firm pushing-turningmotion, and at the instant the 380 mark isreached, start the stop watch noting the timerequired for the mercury column to dropfrom 380 to 360. This figure represents thetime necessary for 10 milliliters of air topass between tbe plane surface and that ofthe test specimen. This is a numerical meas-ure of the smoothness of the sample. Beforeremoving the paper, turn the stopcock clock-wise hack to the “o” position. If the timerequired for the 20-millimeter drop is over300 seconds, turn the stopcock clockwise tothe 1/10 position and multiply the observedtime, for the 20-millimeter drop, by 10. Testat least five specimens for the wire side andat least five for the felt side of the sample.Use separate specimens for each test sincethe pressure on the test specimen compressesthe fibers in the sample.

5. Report

5.1 The average amoothneas in secondsfor not less than five teata on each aide ofthe paper shall he reported.

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Method 1313 MAR(.X 1949

FOLDING ENDURANCE, SCHOPPER

1. Scepe

1.1 This method is for testing the fold-ing endurance of papers not more than 0.01inch thick.

2. Teat specimens

2.1 The test specimens shall be cut ac-curately in each principal direction of thepaper with a width of 15 millimeters (0.59inch) and in a length of 100 millimeters (4inches). They shall be free from folds,wrinkles, or blemishes.

3. Appsratus

3.1 The apparatus shall be a Schoppertype folding endurance tester conforming tothe following:

3.1.1 Two horizontally opposed clamps,approximately 10centimeters apart, providedwith spring tension that varies during thefolding cycle as a slotted folding blade, slid-ing back and forth between creasing rollers,folds the paper. The clamps while in motionare freely suspended between the tensionsprings, except that they are supported frombelow by rollers. The folding blade is 0.50millimeter (0.02 inch) thick, and the edges ofthe vertical folding slot are cylindrical andextend somewhat above and below the nor-mal position of the test spscimen. The fourcreasing rollers, each approximately 6 mil-limeters in diameter and 18 millimeterslong, are arranged symmetrically about themidposition of the folding slot, and are pref-erably provided with jewel bearings.-

3.1.2 A mesns of imparting harmonic

motion of constant period to the reciprocat-ing blade. A power-driven apparatus ispreferable.

3.1.3 A device to register the number ofdouble folds, which stops automatically whenthe specimen bresks.

4 Procedure

Al With the vertical slot of the recipro-cating blade in ita central position, place thespecimen in the slot and fasten the endsfirmly and squarely in the clamps with thesurface of the specimen lying wholly witbinone plane. Handle the specimen by the endsand do not touch it with the hands in the re-gion which is to be foIded. Then apply thespecified tension and fold the specimen at auniform rate of approximately 120 doublefolds per minute until it is severed at thecrease. Record the number of double foldsrequired to sever the specimen.

5. Report

5.1 Resulte shall be reported as Schop-per folding endurance for each of the princi-pal directions of the paper. The folding en-durance reported shall be the average of notless than 10 tests in each direction. Testgrun on strips having their length cut in themachine direction shall he designated ssthose of machine direction, and tests onstrips cut at right angles to the machine di-rection shall be designated as those of crossdirection. In reporting test results, all digitsafter the first two shall be rounded to zero.

liom I.—In detailspecifications,if the kind offoldingendurance is not stated,.it shallbe under-stoodto be Schopper.

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FOLDING ENDURANCE, M. I. T.

/ 7

1. ScOps

1.1 This method is for testing the fold-ing endurance of paper of any thickness.

2. Tsst apecirnsm

2.1 All of the provisions given in 2.1 ofmethod 131 shall apply except that test speci-mens of definite length are not required.They shall he cut of such length as to insurea firm grip in the clamps without buckling.

3. Apparatus

3.1 A loading clamp constrained to movewithout rotation in a direction perpen-dicular to the axis of rotation of the foldinghead specified below and having its clampingsurfaces in the plane of this axis. The loadis applied through a spring attached tO theloading clamp which is easily adjustable ~provide any desired tension on the speci-men from Oto 1.5 kilograms. The deflectionof the spring when loaded shall not be lessthan 17 millimeters (0.67 inch) per kilo-gram.

3.2 An oscillating folding head support-ing two smooth, cylindrical folding sur-faces parallel to, and symmetrically placedwith respsct to, the axis of rotation. Theposition of the axis of rotation should be ap-proximately in the common tangent plane tothe two folding surfaces in the conventionaldesign and midway between them. The fold.ing head is provided with a clamping deviceback of the axis of rotation and so designedthat no clamping pressure is exerted nearerthan 0.375 inch to the bending axis. The ‘ro-tary oscillating movament of the foldingclamp shall be such as to fold the paperthrough an angle of 135° * 5° to both rightand left of the pnsition of zero fold.

3.3 Each of the two folding aurfaceahaa a radiua of curvature of 0.38 & 0.01S

millimeters (0.015 & 0.001 inch) and alength of not less than 19 millimeters (0.75inch). The distance separating the foldingsurfaces shall be greater than the uncom-pressed thickness of the paper being testedbut shall not exceed it by more than 0.25millimeter (0.01 inch).

3.4 A power-driven device for impart-ing a rotary oscillating motion of constantperiod to the folding clamp.

3.S A device for registering the num-ber of double folds required to sever thespecimen.

4 PrOccdure

4.1 Place the oscillating folding head inthe position of zero fold. Place on top of theplunger a weight equivalent to the tensiondesired on the specimen, and clamp the plun-ger in position when depressed under thisload. Then. clamp the specimen firmly andsquarely in the jaws with the surface of thespecimen lying wholly within one plane andnot touching the jaw mounting-plate. Thedistances separating the folding surfacesshall be greater than the uncompressed thick-ness of the paper being tested, but shall notexceed it by more than 0.25 millimeter (0.01inch). Handle the specimen by the ends anddo not touch it with the hands in the regionwhich is to be folded. Then apply the speci-fied tension to the test strip by releasing theplunger. If the reading of the load indicatorhas changed, reset it by means of the adjust-ing screw to agree with the readihg obtainedwhen the weight was applied. Wheneverpossible, a tension of 1 kilogram shall beused, but if this dues not afford practical teatresults, a greater or a lesser tension may bused. Fold the strip at a uniform rate of175 & 25 double folds per minute until it issevered at the creaae. Racord the number ofdouble folds raquirad to sever the specimen.

UU-P-31b


Method 132

5.Report

5.1 Results shall be reported as M. I. T.folding endurance for each of the principaldirections of the paper. The folding endur-ance reported shall be the average of not lessthan 10 tests in each direction. Tests run onstrips having their length cut in the machine

;

UU-P-31b

directionshallbe designated as those of ma-chine direction,and tests on strips cut atright angles to the machine directionehallbe designatedas those of crossdirection.Inreporting test results, all digits after the firsttwo shall he rounded to zero. If the tensionis other than 1 kilogram, the tension usedshall. be reported.


~,._ <--.,,...—-’ ------


MACHINE DIRECTION (GRAIN)

1. Definitions

1.1 The two major directions of paperare termed as follows:

Machine direction.—The direction of pa-per parallel to its forward movement on thepaper machine. This is aleo termed “grain.”

Cross directto?z.-The direction of the pa-per at right angles to the machine direction.

2. Test specimens

2.1 Cut the test specimene with sidesparallel to the major directions of the origi-nal paper sample sheets. Mark the majordirections of both the sample sheets and thetsst epecimens so that they can be respective-ly identified. For the method in 3.1.1, uee apiece approximately 50 millimeters (2 inch-es) square or a circular piece 2 inches in di-ameter, and for the method in 3.1.2, use twostrips approximately 12.5 millimeters (0.5inch) wide and 152 millimeters (6.0 inches)long, cut at right angles to each other.

3. Prncedure

3.1 A positivereeultobtained by one ofthe following methods shall be regarded as aconclusive determination:

3.1.1 Float the specimen on water andnote the direction of tbe curl. The axis ofthe curl is parallel to the machine directionof tbe paper. Paper which absorbs waterreadily should not hc exposed to the waterfor more than a few seconds.

3.1.2 Hold the two strips by the ends ina horizontal position, one over the other,placing first one and then the other on top.The strip cut in the cross direction will bendthe more and fall away from the one cut inthe machine direction.

3.1.3 Burst tbe specimen as described inmethod 112 for determination of burstingstrength. The chief line of rupture will beat right angles to the machine direction ofthe paper.

UU-P+lb


Method 150s MARCR1949

OIL PENETRATION

1. scope

1.1 This method is a meaaure of the re-ceptivity of paper to printing inks having anoil vehicle. It is suitable only for easily per-meable papers such as news, hook, and mime-ograph.

2., Teat specimen

2.1 The test specimen shall be 51 by 51millimeters (2 by 2 inches).

3. Apparatus

3.1 Box having an open front; a ground-glass top containing a 0.75-inch hole for ob-servation of the specimen; a ground-glasspartition parallel with the front side to pre-vent excess heat from affecting the test re-sults; a 15-watt electric bulb placed back ofthe partition for illumination of the sample;and an adjustable mirror near the bottom oftbe box and centered on tbe hole in the top ofthe box for observation of the specimen.

3.2 Separator funnel with a tip approx-imately 0.75 inch in length and of such di-ameter that 25 drops of distilled water deliv-

1 ered at 21”C. (700F.) will have a volume of

I milliliter. The funnel is suspended withthe end of the tip approximately 1.75 inchesabove the test specimen and contains U.S.P.castor oil, the temperature of which is main-tained during the test at 25° & 2“C. (’77° &3.5”F.) .

4. Procedure.

4.1 Place the specimen over the hole inthe top of tbe box. Let a drop of the U.S.P.castor oil fall from the funnel upon the speci-men and start a stopwatch the instant thedrop strikes the specimen. Observe the underside of the specimen and measure the timeinterval from the instant of contact of the oilwith the paper until the spot of oil reach-w auniform and maximum translucency. Cover-ing the spot of oil with a cap having a blackinterior aids in the determination of tbe endpoint.

5. Report

5.1 The report shall state the averagetime of penetration of the oil in seconds totbe nearest 5 seconds, for not less than fivetests on cash side of the paper.

UIJ-P-Slb


1. Definition

1.1 The essential principle of the con-trast-ratio method of determining the opaci-ty of paper which is here specified, is as fol-lows: The apparent reflectance of transhi-,cent paper when combined with a whitebacking is higher than ita apparent reflect-ance when combined with a black hackingbecause of the greater amount of light re-flected from the white backing. The ratio ofthe lower reflwtance to the higher, expressedin percentage, is taken as the opacity of thepaper, this being 100 percent for perfectlyopaque paper and nearly zero for perfectlytransparent paper.

2. Test sp-ens

2.1 The test specimens shall be of suit-able size to tit the holder of the apparatus.They shall be clean and free from folds andwrinkIes.

3. Apparatus

3.1 The standard black backing shallhave an apparent reflectance of leas than 0.5percent. It shall consist of a permanent dif-fusing surface of this apparent reflectance incontact with the sample, or of an equivalentbacking, such as a cavity lined with blackvelvet or other material that will lead to anaPParent reflectance of less than 0.5 percent.

3.2 The standard white backing shallhave an apparent reflectance equal te 91.5percent. It shall consist of a permanent dif-fusing surface of this apparent reflectance incontact with the sample, or of an equivalentcavity, such as that provided by a diffusingsurface separsted from the sample by a coverglass.

Method 1513 MARcH 1949

OPACITY

3.3 Measurements of apparent reflect-ance shall be by light from an incandescentlamp or lamps at a color temperature be-tween 2,400 and 2,800 K (common electricbulbs of 100 watts or less, used at their des-ignated voltage, are usually acceptable), andshall be by illumination which is in effectcompletely diffused. The direction of viewshall be not more than 20” from the normalto the surface of the sample, or equivalentconditions of illuminating and viewing shallbe used, such as unidirectional illuminationat an angle of not more than 20° from thenormal to the surface of the sample and ob-serving all reflected light.

3.4 The holder for the specimen shall beso constructed that the zample is held flat towithin 1 percent of the diameter of the areaused for the measurements.

3.5 Observations shall be by the humaneye or by an equivalent means, such as aphotoelectric cell with a filter adjusting thespectral sensitivity to that of the human eye.

4. Procedure

41 The procedure appropriate to t~eaPParatus shall be used and the results shahbe calculated as a ratio expressed in percent-age and recorded to three significant figures.

5. Report

5.1 The test results shall be reported aa !contrast-ratio opacity, calculated as a per-centage to the nearest 0.5. The opacity of asample shall be tbe average of the resultsobtained from testing not less than five speci-mens.

UU-P-31b


Method 160J MARCH 1949

SAMEWNG AND PREPARATION OF TEST SAMPLESe

1. %pe

1.1 This method isfor sampling sheetorrollpaper and prepm-ing the samples fmtesting.

2. Test eample

2.1 The test sample, unless otherwisespecified, shall consist when possible of speci.mens each cut not iess than 11 by 11 inches.This allows margin for trimming exactly 10by 10 inches,which simplifiesthe calculationof basis weight determination. The speci-mens shallconsistof a sufficientnumber tocompiete tinetests,They shallbe kept smoothand flatand protected from exposure to di.rectsur,light,contactwith liquids,and otherharmf u] influences. Care should bc exercisedin handling the specimens if optical, surface,acidity, or other physical or c“bemical charac-teristics affected by the moisture of thehands are to he determined. In the case ofa test for moisture the test sheets shall beplaced, immediately after sampling, in a canmade airtight by means of a cover and keptin this condition until the moisture test isperformed. When an accurate moisture testis important, it is desirable to take a separatesample for this and weigh the sample beforeopening the contair,er.

3. Procednre

3.1 The specimens comprising the testsample shall he so selected as to be represen-tative of the entire lot of paper. One set ofspecimens shall be taken from one unit outof every twenty in the shipment, except thatthe minimum number of sets taken from ashipment shall be 5 and the maximum num.

her 20. The same number of specimens shallbe taken from each unit. The units shall. herolls. cases, frames, skids, or bundles.

3.2 In the case of ‘rolls, special care shallbe taken to select test sheets that are notdamaged. It is good practice, where mois.ture iS not important, to discard the fir.gtthree layers of the roll to be sure of obtain.ing a unit sample in good representative con-dition. When the moisture is to be deter-mined, the sample shall not be taken within% inch Of tbe outside of the roll. The speci-mens shall be cut from sheets talcen acrossthe full width of several unharmed layers.

3.3 in the case of sheet-cut paper,specimens shall be cut from at least five con-secutive sheets taken from a p~int or pfiintsover j~~inch from the top or bottom of eachcase, frame, skid, or bundle sampled.

3.4 The specimens shall be trimmed withtheir edges exact!v Darallel to the machineand cross directions of the paper.

3.5 A autlicient number of specimensfrom each unit sample shall then be arranged ●consecutively in rotation to form a represen-tativetestsample. A convenient way to dothis is to number consecutivelythe sheetscomprising each set and then selectsheetsbearing consecutive numbers, one or morefrom each set, in rotation.

4. ResampIing

4.1 In case of necessity for resamplinga lot of paper, the samples shall be taken asdescribed above, except that the samplesbeeta shall be taken from units differentfrom those previously sampled.

UU-P-311)


Method 1703 31ARCH 1949

TE.4RING RESISTANCE

L Scope

1.1 This method is adapted for deter-mining the force in grame required to teara single sheet of paper after the tear hasbeen started.

2. Test specimene

2.1 Specimens for the test shall be cutaccurately in each principal direction of thepaper about 76 millimeters (3 inches) longby exactly 63 millimeters (2.5 inches) wide,with the slit to be cut 20 millimeters long,leaving exactly 43 millimeters (1.69 inches)between the end of the slit and the edge ofthe specimen.

3. Apparatus

3.1 The apparatus shall be an Elmendorftype of tester conforming to tine following:

3.1.1 The test apparatus shall have: (1)a stationary clamp and a movable clamp car-ried on a pendulum, preferably formed by asector of a wheel or circle, free to swing Ona ball or other substantially frictionless bear-ings; (2) a pointer and pointer stop to re-cord the maximum arc of swing of the sectorpendulum; (3) a sector release to hold tknependulum in tbe raised position during themounting of the sample, and permitting it tofall through the force of gravity; (4) a pen-dulum carrying a circumferential graduatedscale so as to indicate the force used in tear-ing the specimen; (5) a knife attachment forinitial slitting of the specimen.

3.1.2 With the pendulum in the raisedposition, the movable clamp shall lie in thesame plane as the fixed clamp forming as itwere an extension to the fixed clamp. Thisplane sM1 be perpendicular to the plane ofoscillation of the pendulum. The grippingsurface of the jaws in each clamp shall be25 millimeters (0.984 inch) by 16.5 milli-meters (0.650 inch). The clamps shall be

separated by a distance of 2.5 millimeters(0.098 inch). The knife attachment shall slitthe specimen midway between the clamps atright angles to the upper edge of the clamps.The slit shall extend from the bottom edgeof the specimen to a point 4 millimeters(0.157 inch) abo~~e the top edge of theclamps leaving a distance of M millimeters(1.692 inches ) of uncut specimen perpendic-ular to the !ong dimension of the specimen.The perpenri;cula? from tbe line formed bythe top edge of the clamps to the axis of sus-pension shall be 104 millimeters (4.09 inch-es) and shall make an angle of 27.50 witlnthe plane of the specimen.

4. Procedure

4.1 The specimen shall be placed secure-ly in the clamps. BY use of the knife biade aslit shall be cut in the specimen starting atthe bottom edge and perpendicular thereto,and ending 43 millimeters (1.692 inches)short of the top edge. The accuracy of thereadings obtained with the apparatus de-pends to a great extent on the exactness ofthis 43 millimeters of uncut epecimen. Thesector release shall be pressed, causing thesector to fall, thus moving the pendulum jawaway from the fixed jaw so as to tear thespecimen. The force required to tear tbe spe-cimen in the given direction shall he readfrom the scale. Readings obtained where thetear deviates more than 10 millimeters (%inch) away from the line of ths initial slitshall be rejected. Likewise if the side of thespecimen above the movable jaw rubs againstthe sector as the tear is made, the readingshall be rejected.

4.2 The test shall be made on enoughsheets so that when torn together, the sealsreadings are between 20 and 6Q, and thenumber of sheets used shall be recorded. Notless than five tests shall be made in eachprincipal direction of the paper.

UU-P-31b


Method 170

5. Report 16 and dividing by the number of sheets torn

5.1 Report the results as the average at one time. Report the results obtained on

force in grams required to tear a single strips torn in the machine direction as tear.

sheet. Since the scale readings are made 1/16 ing resistance, machine direction, and on ●of the actual’values, this iscalculated by nru1. strips torn across the machine direction as

tiplying the average instrument reading by tearing resistance, cross direction.

%

UU-P-31b


Method 171,3 MARCH1949

TENSILE BREAKING STRENGTH (DRY) ANDELONGATION

L Scope

1.1 This method is for the measurementof the dry tensile strength of all weights ofpaper and paperboard.

2. Test specimens

2.1 The specimens for test shall be stripscut accurately and with the sides parallel.The length shall he not less than 140 milli-meters (5.5 inches), and the width shall be15 millimeters (0.5 inch), except that forheavy papers and paperboards, the widthmay be 25 millimeters (1 inch) or 51 milli-meters (2 inches).

3. Apparatus

3.1 The tensile testing instrument shallconform to the following:

3.1.1 Two clamps whose centers shall bein the same plane parallel with the directionof motion of the stressing clamp and soatigned that they will hold the test specimenwholly in one plane.

3.1.2 A pendulum so attached to oneclamp as to balance the load applied to thespecimen accurately, with a device to indi-cate on a graduated scale the breaking loadof the test specimen.

3.1.3 A means of moving the stressingclamp at a uniform rate.

.4.. Procedure

4.1 The ratio of the clearance distancebetween jaws to the width of the specimenshall be not less than 5:1, nor more than12:1. The test specimen shall be firmlyclamped squarely in the jaws of the clamps,

and the stressing jaw then operated at aspeed of 30.5 centimeters (12 inches) perminute until the specimen breaks. Thebreaking load shall be recorded to the near-est 2 percent of tbe total indicated reading.The tester shall be of such capacity that thetensile strength of the paper tested will benot greater than 90 p+rcent nor less than 10percent of the capacity of tbe tester. Notless than 10 strips cut in each principal di-rection of the paper shall be tested. All thereadings obtained when the paper breaks ator in tbe jaws shall be rejected. Elongation(or stretch) shall be measured at the instantof rupture of the specimen, either by meansof a recording device attached to the ma-chine, or by measuring between referencemarks on the specimen with a scale. Not lessthan 10 specimens shall be tested. Whenelongation is to be measured, care shall betaken to apply no more initial tansion to thetest strip before clamping it than is requiredto straighten it.

5. Repori

5.1 The average of the test results shallbe reported for each of the principal direc-tions of the paper in kilograms per 15 milli-meters width, or pounds per inch width, tothe nearest 2 percent of the totil reading.Test results of atrips cut in the machine di-rection of the paper shall be reported as ten-sile breaking strength, machine direction,and test results of strips cut across the ma-chine direction shall be reported as tensilebreaking strength, cross direction. The av-erage of the elongation test results shall bereported as a percentage of the length of thestrips between the clamps to the nearest 1.

uu-P-31b


.Method 1723 MARCH 1949

TENSILE BREAKING STRENGTH, WET

1. scope

1.1 This method is for the determinationjf the tensile breaking strength of paper andpaperboard after they have been wetted wi kbwater or other liquid.

2. Teat specimens

2.1 The specimens for test shall be asspecified in method 1.71.

3. Apparatus

3.1 A tensiletesteras specifiedin meth-od 171.

3.2 A Finch wet-strengthattachment forthe tensiletester. The device consistsof aatirrwp about 1.5 inches -wideand 3 incheslong, made of two metal straps which r,up-port horizontallya cylindricalrod,3/16 inch

(5 mm.) in diameter and a littlemore than1 inch long. Iletw-eenthe strape is a smali

verticallymovable container for hokiing wa-ter or other liquid. The liquid coxtainerlocks in its uppermost positimr, so that thehorizontal rod is immersed in the liquid toa depth of at !east 0.75 inch. A metal tongueat the bottom of the stirrup permits it to beclamped in the lower jaw of a tensile tester.

4. Prncedure

4.1 Immerse the test suedmens h tineliquid for the lengthdetail specification.

of time stated in the

42 Use the Finch device for wetting tis.sue papers, paper towels, and other papersthat are difficult to handle when wet.’ C!arcpthe device in the lower jaw of the tensiletester. Place the liquid container in its low-est position and nearljj till it with the liquid.I.oop the dry test specimen under the dryhorizontal rod and clamp the two ends of thespecimen in the upper jaw of the tensile test-er. Raise the liquid container so that it locksin its uppermost position, thereby immersingthe looped end of the specimen to a depth ofat lesst 0.75 inch. At the end of the immer-sion period, proceed with the test with tneliquid container in its uppermost position.The indicated strength is divided by 2 to ob-tain the wet strength of a single strip.

4.3 To wet materiala that can be han-dled without difficulty when wet, and paper-

+

boards, wholly immerse each test strip in ashallow dish of liquid. After the predeter-mined time of wetting, withdraw the atrip,iay it flat and straight on a pad of blottingpaper, cover with a sheet of blotting paper, ●and pass a 500-.gram cylinder over the cover,taking about 1 second to complete the rolling.

4.4 The test shall be made in accordancewith the procedure given in method 171.

5, Repori

5.1 The results shall be reported as ape

cified in method 171.

UIJ-P-31b ;

●



THICKNESS

1. Scope

L 1 This method s~all be used for deter-mining the thickness of a single sheet of pa-per or paperboard as it would measure whsnplaced between plane surfaces.

2, Tast r.pecimen

2.1 Whenever possihie the test speci-men shall be not less than 51 by 61 milli-meters (2 by 2 inches). It shall be free fromwrinkles and creases.

3. Appammm

3.1 Microm.eter.—The micrometer usedshall be in accordance with the following re-quirements:

3. L 1 It shall have two plane faces, thesmaller of which is circuiar and 0.25 to 0.33square inch (160 to 215 sq. mm. ) in area,corresponding to a diameter of 0.56 to 0.65inch (14.3 to 16.5 mm.). The faces shall hepsrallel to within 0.0002 inch (0.005 mm.)and constrained to move apart in an axisperpendicular to themselves.

3.1.2 When the specimen is clamped be-tween the faces, it shall be under n steadypressure of 7.0 to 9.0 pounds per square inch(0.40 to 0.63 kg. per sq. cm.).

3.1.3 The distance between the gradua-tions on the dial shall be snch as to permitof estimating the thickness to at least 0.0001inch.

3.1.4 The micrometer shall be such as torepeat its readings to within 0.0001 inch atzero setting or on a steel gage block.

3,1.5 Measurements made on standardsteel thickness gages shall be within the fol-lowing tolerances of permissible deviation ofthe reading from tbe actual thickness of tbestandard steel gage:

IIntervals Tolerance

.wWmet.,, 1 =-l=-i. wtetera

0 to0.25 to0.01 0.9025over 0.25to1.02 0.01to0.04 0.0051Over 1,02to3,05 0,04to0.,2 I 0.0,0,

— I_ 1,

3.2 Cal.ibrucion.

Inch

0.00010.00020.0004

3.2.1 Parallelism of the faces.—A hardsteel ball about 1/16 inch in diameter, fixedfirmly in a thinner flat piece of metal to serveae a handle, shall be placed at different pointson the anvil and the readings noted.

3.2.2 Accuracy of the readings.-The in-strument shall be eet to zero and standardgagee shall be placed between the plane facesand the correspocdi~g dia! readings observedover the range to be ueed. For thicknessmeasurements, standard steel gage blockshaving an accuracy of 0.00001 inch shall beueed.

3.2.3 Pres8wre between the faces, -—Theforce required to just prevent the movementof the plunger foot, from a reading corres-ponding to about the average paper thicknesstested to a lower reading, shall be deter-mined with a suitable balance, and tbe con-tact pressure determined with this force.For example where the pressure foot pro-jects through the top of the apparatus, a finecopper wire is attached to it and by meansof a coarse balance or a calibrated spring,the force necessary to prevent the closing ofthe foot is measured.

3.2.3.1 Alternatively, a stirrup may beused, made of a flat metal plate having a holelarger than the diameter of the micrometerfoot, covered at tbe bottom of the plate by athin metal disk of about the average thick.ness of the paper to be measured. The stir-rup is suspended from a suitable balance.

UU-P-3 lb


Method 173

4. Procedure sheets shall be tested in not less than two dif.

4.1 Place the specimen between the jawsferent places.

of the micrometer and lower the pressure 5. Repotifoot. gently upon the surface of the paper atleast, whenever possible, 0.25 inch (6 mm.) 5.1 The thickness shall be reported as anfrom the edge of the paper, and record the average of the test results in decimals of anreading on the dial, Each of 10 different inch to the nearest 0.0001 inch (0.002 mm.).

UU-P-31b



\

WATER ABSORPTIVENESS

/ L scope

~ 1.1 This method is applicable te paperhaving a fairly rapid rate of absorption of

~water such as @per toweling and other tis.i sue papers.

2. Test epecfmens

2.1 Each test specimen shaI1consist ofa single sheet approximately 4 inches square.

3. Apparatus

3.1 A l-milliliter measuring P@tegraduated in hundredths of a milliliter, orthe Carson microhurette. (For informationon the latter consult National Bureau of.%mdards Research Paper RP959.)

3.z A 4.mesh wire screen.

4. Procedure

41 Place a specimen on the screen andfill the pipette or microburette with distilledwater having a temperature of 23” & 2“C.

(73° + 3.5”F.). With the pipette or micrO-burette at an angle of about 30° with thehorizontal, and with the tip nearly in contactwith the paper, allow a measured amount ofthe water to flow on the specimen near itscenter. While the water is flowing, keep thetip in the drop of water until delivery of thewater is completed. The amount of water de-livered shall be as stated in the detail specifi-cation. If the time of absorption is morethan about 2 minutes, cover the water on thepaper with a watch glass. Measure with astopwatch the rate of absorption in secondsfrom the start of flow of water until the dropof water is completely absorbed as indicatedby no further reflection of light from it whenviewed at an angle. An equal number oftests shall be made on each side of the paperand not less than 10 specimens shall betested.

5. Report

5.1 The report shall state the average ofthe test results in seconds.

BUU-P-31b



WATER RESISTANCE

L Scope

1.1 Thismethod,termedthedry-indica-tormethod,isfortestingthetimeofpermea-tion of water through papers and paper-boards.

2. TeOt specimene

2.1 Whenever possible the test speci-mens shall be about 64 millimeters hy 64millimeters (2.5 inches by 2.5 inches). llneyshall be free from folds, wrinkles, or otherblemishes not commoni:; inherent in the ma-terial.

3. +pamtus

3.1 A vessel of water of sufficient sizefor floating several specimens simultaneous-ly, immersed in a water bath in which thetemperature of the water in the vessel canhe maintained 8). 23” & 0.50C. (73” &l’F. ).

4. Indicator

4.1 The dry indicator shall he made ofpure cal>e sugar, pure soluble starch, andmethyl violet, as follows: Grind each in-gredient separately until it passes througha No. 100 screen, and completely dry it in adesiccator over CaCl, hefore making the mix-ture. When dry, weigh .md mix the follow-ing proportion by weight:

Sugar 45Solutile starch 5Dye 1

Mix the ingredients by screening repeated.

b’ thrOugh a No. 60 screen until the mixtureis uniform, Keep tine indicator in a desic-

cator when it is not being used.

5. F%occdure

5.1 The indicator reagent shal! be aprin-Ided evenly over’ approximately a Z-inch-square area (l-inch for 2- by 2-inch sveci-mens } in the center of the aampie. Careshould be taken to app~y this reagent asevenly as possible since bunching or pilingof the reagent causes different values. .42-inch watch glass (l-inch for 2- by Z-inchspecimens) issealed over the indicator pow.der using a mixture of 50 percent beeswaxand 50 percent rosin. The edges shall beturned tip or dipped in wax to prevent con- $

tact of the water with the adhesive and thespecimen tioated on tap water maintained at23” * 0.5°C. (73° * l°F. ). The time re-quired for a definite development of color toappear in the indicator shall be noted and re.corded as the penetration time. Make at ●least five tests from each side of the mate-rial.

6. Repori

6.1 The water resistance shall be the

average of all test results reported in min-utes or hours.

UU-P-31b


Method 1823 MARCH1949

WATER VAPOR

1. 8cOpe

1.1 This method is for testing the watervapor permeability of paper, paperboard,and other sheet materials.

2. Test specimens

2.1 Each test specimen shall be a circleof the imaterial and ehall be not less than 3inches in diameter.

3. Apparatus

3.1 An open-mouthed C.UPor dish of suchsize and shape that it can be accommodatedreadily on the pm] of an analytical balance.‘lUe opening should be as iarge as practical,an area of at least 50 square centimeters be-ing preferred. (This is equivalent to a circleabout 3 inches in dismeter. ) The test dishshall be of such desigu that a wax seal canbe made which will bs impervious to leakageof water vspor and will define clearly thetest area.

3.2 A template for nse in defining thetest area and effecting the wax seal, cm]sist-ing of a circular metal disk ~3 to 1A inchthick, with the edge bevelled to an angle of3bout 45”. The diameter of the bottom(smaller) face of the template shall not begreater than the diameter of the eiTectiveopening of the cell in contact with the speci-men.

3.3 An analyticrd balance of 200-gramcapacity, sensitive to 0.001 gram, with panslarge enough to hold the test dish+.

3.4 A testing room or cabinet whereinthe circulating air can be maintained ateither 50 * 2 percent relative humidity and23” * 2“C. (73” & 3.5”F. ), or at 90 & 2 per-cerlt relative humidity and 38” + 2“C. (100°& 1“F.). The room or cabinet shall havesuitable grills or racks to support the assem-bled specimen dishes, with means for circu-lating the conditioned air continuously over

PERMEABILITY

the entire ex~osed area of the test specimerm.In testing at the higher humidity and tem-perature, the design of the room or cabinetshall be such as to avoid condensation in thevicinity of the test specimens, and if it is~,we~sar.vto ~emok.ethe test ~Pwimen ~s~e.-

blies from !be room or cabinet for weighing,tight c.ovsrs must be provided for the twtdish.w.

4 Procedure

4.1 Use as a desiccant, wrhydrous calci-um chloride in the form of small lumps, freefrom fines, that will pass a No. 30 screen.Place sufficient desiccant inside the dish tocover the sheet area evenly to a depth ofabout 15 millimeters.

4.z The following method ofafixing thetest specimen to the dish is for paper andfor paperboards not ever Y8 inch thick: Cutthe test specimen so that its diameter is egualto that of the Parger diameter of the temp-late. Place the sheet over the aperture ofthe dish and center it as closely as possfoleon tine supporting ring or flange. With tinetip of the finger apply a thin film of petrO-lati~m to the bevelled edge of the template.Wipe otT any petrolatum which may havebeen deposited on the smaller surface of thetemplate. Center the temukte, with thesmaller surface down, exactly over the speci-menand dish opening. Flow molten wax’intothe annular space surrounding the bevellededge of the template, usinga medicine drop-pertodispense the molten wax. Remove thetempk.te from the sheet surface as soon asthe wax has cooled and solidified. The waxshall consist of a mixture of 60 percent amor-phous wax and40 percent crystalline paraf-fin wax.

4.3 For paperboards over % inch thick,the method of preparing the test assembly ismodified as follows: To prevent edge leak-age, rotate the edge of the test specimen in

ULJ-P-31b


Method 182

molten wax of such fluiditythat itdoes notpenetrateintothe edge more than 1/16 inch,suspend it inside the dish to a distance ofabout half the thickness of the specimen, andrun molten wax around the edge of the speci-men to seal it to the dish.

4.4 Weigh the assembly on the analyti-cal balance to 0.001 gram. Place the dish onthe rack inside the testing room or cabinetin an inverted position so that the layer ofdesiccant is in direct contact and evenly dis-tributed over the inner face of the test sheetand so that free access of the conditioned cir-culating air is provided on the exposed sur-face of the sheet.

4.5 The atmosphere of the testing roomor cabinet shall be maintained during thetesting at either “50 & 2 percent relative hu-midity and 23° * Z“C., or 90 + 2 percentrelative humidity and 38° & Z“C., as speci-fied in the detail specification.

4.6 Make successive weighings of the as-

sembly at suitable intervals until a constantrate of gain of weight is attained. If thedishes are weighed in an atmosphere differ- ●ent from that of the testing atmosphere, theyshall have tightly fitting covers during theweighings. For papers that are relativelypervious, the weighings should be frequentenough to complete the test before drops ofliquid agglomerate are formed in the desic-cant or caking of the desiccant occurs. Theseconditions will he indicated by a drift fromthe constant rate of gain. At least four speci-mens shall be tested, with an equal numberof each side exposed to the higher humidity.Plot the gain in weight against time. Theslope of the resulting curve will furnish ameasure of the water vapor permeability.

5. Report

5.1 The water vapor permeability shall bereported as an average of all test results totwo significant figures as grams per squaremeter per 24 hours. The calculation shall hemade for the period of constant rate of gain.

UU-P-31b


Method 183t MARCH 1949

WIRE AND

1. Scope

1.1 The wire side of paper. is the sidethat was in contact with the wire of the papermachine; the other side is termed the feltside. It is desirable to have means of distin-guishing between thetwosides because theygenerally differ in some physical character-istics. It is not always possible to make thedistinction, this being particularly true ofcoated and other surface-treated papers, cer-tain’ high-grade papers made from well beat-en rag stock, and specialties made with vari-ations in the usual paper-machine practice.When one of the following procedures doesnot give a definite indication, it is advisableto try one or more of the other procedures.

2. Procedures

2.1 Fold over a sheet of the paper andobserve the relative smoothness of the twosides. Often the pattern of diamond-shapedimpressions of the machine wire can be seen,thus identifying the wire side. In viewingthe paper, it should be held in a horizontalposition with the light striking it at an angleof about 45° and with the line of vision ofthe eye also at an angle of 45” to the surfaceof the paper. Observation with a microscopeis helpful.

2.2 Dipthe paper in water orin a weakcaustic soda solution, drain off the excessliquid, allow to stand a few minutes, andagain examine the two sides. This treatmenttends to restore to paper the texture it hadon the machine wire. View as described in2.1.

2.3 Hold asheetof paper inone handinsuch a way that the grain (machine) direc-

FELT SIDES

tion is parallelto the line of vision and thesheet surface is approximately horizontal.Holding the sheet in this position with onehand, pull upward with the other to start atear in the sheet so that the line of tear fol-lows the grain of the paper. As the tear isbeing made, gradually guide it so that itmoves in the cross direction and toward theouter edge of the sheet, producing a tear Iinefollowing a curved path. Turn the sheet overso that the opposite side is uppermost andmake a similar tear in the sheet. Observe thefeatbering caused by the splitting of thesheet at the edge of the two tears which havebeen made. One of theee tears will show adistinct feather edge as compared to theother, especially in the curved portion wherethe line of tear departs from the grain ormachine direction and moves toward thecross direction. The tear with the morefeathered edge is always made when the wireside of the sheet faces upwards.

2.4 Cut specimens approximately 1 inchwide and 2 inches long, with the long dimen-sion at right angles to the machine directionof the paper. Place the specimens in a dry-ing oven at approximately 1000C. or in adesiccator over a suitable drying agent, suchas anhydroue calcium chloride. It is essentialthat both sides be exposed alike to the dryingair, and they must be suspended or other-wise held so that they can curl without re-straint. The direction of curl under theseconditions will furnish a reliable means ofdistinguishing between the two sides of mostpapers. On drying, any pronounced curl ofthe specimens will be toward the wire sidewith the axis of the curl parallel to the ma-chine direction of the paper.

UU-P-31b



ACIDITY, p~i

2. Definition

1.1 In this method the PH value of apaper refers to its acidity or alkalinity interms of hydrogen ion concentration of theunfiltered aqueous extract of the cut orground paper.

2. Test Opecimen

2.1 The test specimen shall consist of 1gram of air-dry paper. Ordinary paperasuch aa bond and writing may be tested intineform of smail cuttings. Paper more than0.012 inch thick or very dense paper shali bereduced to a fluffy form by a disintegrator.

3. Apparatus

3.1 The special apparatus required forthis test is a circuit including a glass eiec-trode and a saturated KCLcalomel half-celicapable of precision to within 0.1 PH. Thecomplete apparatus is commercially avail-able. ‘The apparatus used shall be .gtandard-ized frequently against 0.05 M pGtissiumacid phtha.late solution which bas a pH of4.0 over the entire range of room tempera.ture.

4. Distilled wsier

4.1 For making the extraction, watercontaining ordinary znrmmts of CO,, but notmore than ccrrespouds to a pH of 5.9, maybe used to test all papers, including those inthe neutral range between pH 6.0 to 7.0. Asample of the water must be tested for alka-line impurities, however, by boiling for a fewminutes, cooling, and then measuring itsPH. If this is found to be higher than 7.3,the water must be distilled from a solution

containing approximately 1 gram of KMnO,,and 4 grams of NaOH per liter. A doublestilLhead ia usually necessary.

5. Procedure

5.1 Weigh 1.0 gram. of the air-dry cut mground paper into a 125-nrilliliterErien-meyerflask.Add about20 millilitersofdis-tilled water and macerate with a flattenedstirring rod until the specimen is uniformlywet. Then add 50 milliliters more of the wa-ter, stir,and affixto the flask a stopper con-taining a glass tube about 9 millilitersin di.ameter and 75 centimeters in length, whichserves as a condenser. A soil-digestion flaskwhich has a ground-glass stopper and con-densing tube in one piece, or a rubber stop-per covered with clean metal fail may beused. ?lace tbe flask in a steam bath whichwill maintain the contents of the flaak at 95°to 100”C. without boiling the water. Heat atthis temperature for 1 hour with occasionalshaking, then COOIto 20” to 30° C. (68” to86° F.), and measure the pH of the unfil-tered mixture with the glass electrode. If theglass e!ectrode bad just previously been usedfor measurements in the alkaline region, andif the paper to be tested is in the neutralregion, immerse the electrode in 0,05 M po-tassium acid phthdate for 1 minute and rinsethoroughly several times with distilled waterbefore use.

6. Report

6.1 The PH value of the paper shall bcthe average of duplicate determination:which agree within 0.1 PH. The averag(shall be expressed to the nearest 0.1 PH.

W-P–3 lb


Method .2013 MARcn 1949

ALPHA CELLULOSE

1. Definition nnd scope

1.1 Alpha cellulose is that portion of theceliulose of paper fibers that is insoluble ina strong solutiou of sodium hydroxide underdefinitely prescribed conditions. It is momstable than the modified forms of celluiosethat are dissolved by sodium hydroxide. Itis suitable for all kinds of papers.

2. Test specimen

2.1 A sufficient amount of the paper forthe tests shall be reduced to cotton-like formiri a disintegrator and then thoroughlymixed. Zach test specimen shall weigh 0.3gram.

3. Apparatuo

3. I The special apparatus required forthis test is as follows:

3.1.1 A disintegrator which will com-pletely disintegrate the paper without hatt-ing or contaminating it. A Koerner type orita equivalent shall be used.

3.1.2 A water bath which ean be main-tained at 20” & O.l”C. (6S0 * Z“F.).

4. Reagcnta

4.1 Sodium hydroztte solution, 17.5 pcr-certt (J.24 IN.).—AIIow a 50 percent solutionof C.P. NaOH to stand about 1 week in astoppered vessel to permit settling ofNa,CO,. Draw off 2.00 milliliters of the.vupernatant liquid with a pipette; add about50 milliliters of distilled water and 1 milliliterof 1.5 M BaCl, solution to lessen the effect ofCO, on the endpoint; and titrate with stand-ard 1 N hydrochloric acid, using phenolph-thalein as indicator. Knowing the approxi-mate normality of the concentrated NaOH,dilute it with distilled water to 5.24 & 0.03N, checking the diluted NaOH hy titrating10.00 milliliters of it as before, and dilutingfurther, if necessary, to obtain the normalityspecified, which will correspond to a strength

of 17.”5 & 0.1 percent. (The final so!utionshould have a deusity of 1.194 & 0.001 at15” Cl, or 1.192 * 0.001 at 20”C. )

4.2 Potassium bichromate solution.—-Dis.solve 90.0 grsms of C.P. moisture-free (100”-105” C.) K, Cr,O, in hot water (70°-900 C.)and dilute to 1 liter after allowing the SO!U.tion to cool.

4.3 Ferrow ammonium .Mpltate sokL-tion.-–Dissolve195 grams of C.P. Fe (NH,),(SO.),6H,0 in water containing10 rniililitersof concentrated H, SO. and diluteto 1 li’kw.If the solution is kept out of contact withoxygen, by a slow, continuous stream of ky-

drogen, for example, its st?ength wiil remainquite constant. The amount of H, thus usedis about one fifth of a 200-cubic-foot cylin-der per year. This is not uecessary but re-duces the frequency with which the bichr~-rnate-ferrous ammonium sl?lphcte ratio mustbe determined from daily to two or threetimes monthly.

5. Pmccdure

5.1 Perform all operations described in5.2 and keep all liquids, as nearly as possible,at 20.0” * O.I”C.

5.2 Weigh 0.3 gram * 10 milligrams ofthe specimen in a 100-rnilliliter beaker. Add20.0 milliliters of 17.5 percent NaOH solu-tion, macerate until the fibers are uniformlywet and dispersed and let stand 10 minutesfrom the time of addition of HaOH. Thenadd 33.0 milliliters of water, stir the mixturethoroughly, and let stand 1 hour longer, stir-ring once during the interval. After stirringonce more, pour about 5 milliliters of the un-settled mixture on an 80-mesh copper orbrass wire screen fitted into a Gooch cruci-ble. The crucible and ring are supported bya funnel fitted into the neck of a 100-milli-liter volumetric flask with a rubber stopperthrough which passes a glass tube for suc-tion. Form a mat with gentle suction (pres-

UU-P-3 lb


Method 201

sure differential 10 to 20 mm. of Hg). Avoidexcessive packing of the fibers as this re-tards filtering. It may be necessary to re-filter the first filtrate, but loss of smallamounts of alpha-cellulose to the filtrate doesnot affect the results appreciably. Pour theremainder of the mixture on the mat, and,before the last of the liquid has run through,wash the beaker and the mat with 35 milli-liters of water.

5.3 Moisten the residue of alpha-cellu-lose with water and remove it from the cru-cible. Place the crucible upright in a 400-milliliter beaker, fill it with 25 milliliters of12 M H,SO,, at room temperature, and rinseit after a few minutes with 50 millilitersmore of the acid. Disintegrate the alpha-cel-lulose pad in the acid, using a thermometeras a stirring rod. Add to the alpha-cellulosesolution, with a pipette, 25.00 milliliters ofthe bichromate solution and heat at 140° to150° C. for 10 minutes. Bubble air in a finestream through the solution to preventbumping, and keep the beaker covered witha watch glass notched to permit entrance ofthe thermometer and the bubbling tube.

5.4 After the solution has cooled to130° C., and 50 milliliters of water, rinse thethermometer, etc., and cool the solution to60° C. or lower. Titrate the remaining bi-

chromate with the ferrous ammonium sul-phate solution.

5.5 Pi pet exactly half of the filtratefrom the alpha-cellulose, after all fibers pres-ent have settled, into a 400-milliliter beakercontaining 5.0 milliliters of the bichromatesolution. If the paper contains oxidizablefillers such as ZnS pigment Or CaSO,, filter

—.

the filtrate once through a thick pad of as-bestos in a Gooch crucible before taking theportion for analysis. (Such fillers remainingwith the alpha-cellulose may cause some er-ror, but this is usually slight. ) Cautiously ●and with constant stirring, pour 50 milli-liters of concentrated H,SO. down the side ofthe beaker containing the portion of the fd-trate, then heat and titrate as before.

5.6 The amount of bichromate solutionconsumed in milliliters is calculated for eachfraction as follows:

(a) For alpha fraction, mL=25-(V, x r)(b) For filtrate, ml.==2 (5 V,xr)

where V, and V, represent the volumes offerrous ammonium sulphate necessary to ti.trate the bichromate remaining after oxida-tion in the two cases, respectively, and r isthe volume of bichromate solution equivalentto 1 milliliter of ferrous ammoniuin wdphatesolution, determined frequently by titrating5 milliliters of bichromate solution in 100milliliters of 1:1 H,SO.. The alpha-cellulosepercentage of the total cellulose is calculatedfrom the volumetric data by substitution inthe following equation:

(a) x 100Alpha-cellulose, percent =

(a) + (b)

6. Report

6.1 Alpha cellulose shall be reported asa percentage of the total cellulose, and shallbe the average of duplicate determinationsthe results of which agree within at least0.4. The average shall be expressed to thenearest whole percent.

3(

UU-P-31b


Method 2023 MARC! I 1949

ASH

1. scope1.1 This method is for the determination

of ash, which is defined as the residue aftercomplete combustion of paper and paper-board.

2. Teat specimen

2.1 The test specimen shall consist ofsmall pieces of paper so selected as to be rep-resentative of the sample. Its total weightshall not be less than 1 gram.

2.2 The specimen shall be dried to con-stant weight at 100° to 105” C. and weighedto the nearest 1 milligram. This may be donewith sutlicient accuracy for the purpose inthe ignited and weighed crucible used for theashing of the paper.

3. Apparatus

3.1 A crucible, such as platinum, alun-dum, porcelain, or silica, which does notchange in weight under the ignition condi-tions, and having a tightly fitting lid, is usedfor the ignition.

3.2 An electric mrdfie furnace with anoperating temperature of about 925° C.(1,700° F.) is recommended, but a gas burn-er yielding a similar temperature is also suit-able.

4. Procedure

4.1 Ignite the specimen in the crucible,which; together with the cover, has previ-ously been ignited and weighed to 0.1 milli-gram. To avoid leas of small particles, the

crucibleshalI be covered during the initialignitionof the paper, which shallbe done atlow temperature, and the temperature shallthen be gradually raised to a maximum ofabout 925° C. (1,700” F.). After this tem-perature is reached, the lid of the cruciblemay be slid to one side until tbe combustionis complete. Care must be taken at all timesto protect the contents of the crucible fromair drafts. When the paper is completelyburned, as indicated by absence of black par-

tiCle%remove the covered crucibleto a desic.cater and letitremain untilitstemperatureis in equilibrium with that of the surround-ing atmosphere. Weigh the crucible and con-tents to tbe nearest 0.1 milligram. Repeatthe ignition and weighing until the weightis constant.

4.2 The percentage of ash shall be com-puted on the basis of the weight of the speci-men when dried to constant weight at 100”to 105° C. and shall be the average of at leasttwo determinations. The results should agreeto within 0.1 for papers containing 5 percentash or less, to within 0.15 for papers con-taining from 5 to 10 percent ash, and towithin 0.2 for papers containing over 10 per-cent ash.

5. Report

5.1 The percentage of ash shall be re-ported to the nearest 0.05 for papers contain-ing 5 percent ash or less. For papers contain-ing 5 to 10 percent ash it shall be reportedto the nearest 0.1, and for paper containingover 10 percent ash to the nearest 0.2.

UU-P-31b


Method 220S MARCH 1949

COPPER NUMBER

3.1.2 A steam or oil bath which can bemaintained at 100” C.

4. Resgente

4.1 Copper mdphate soluttin.-—Dissolve100 grams of CUSO.5H,0 in water and diluteto 1 liter.

4.2 Carbonate bicarbormte solution. —Dissolve350 grams of Na,Co,.10H,O (or 129grams of anhydrous Na,CO,) and 50 gramsof NiaHCO, in water and diluteto 1 liter.

4.3 Molvbdophosphoric acid. -Dissolve100 grams of sodium molybdate, Na,Mo04.-2H,0, and 75 milliliters of phosphoric acid(83percerit) ina mixtureof 275millilitsrsof concentrated H, SO. and 1.75 liters ofwater.

1. Definition and scope

1.1 Copper number of paver designatesthe amount of copper precipitatedas cuprousoxide by the celluloseunder definitelypre-scribed conditions. It is a measure of theamount of unstable modified forms of cellu-lose present and thus is related to the stabil-ity cf papers. It is suitable for ail papersexcept those containing zinc sulfide, which isusually a component of zinc pigments.

2. Tmt specimen

2.1 A sufficient amount of paper fcm thetests ehall be reduced to cotton-like form ina disintegrator and then thoroughly mixed.Each test specimen shall weigh about 1.5grams.

3. Apparatus

3.1 The special apparatus required forthis test is as follows:

3.LI A grinder which will completelydisintegrate the paper without heating orcontaminating it. The grinder shaIi be aKoerner type or its equivalent.

4.4 .%dium Carbom.$e solvtion.-An ap-proximately 5 t:ercentsolutionof Na,CO, inwater.

4.5 Potassium permunganate sOluii~a,—0.05 N: 1.5815 grams per liter,

5. Procedure

5.1 Allow the specimen to come to mois.ture equilibrium with the atmosphere of thebaknce. Weigh about 1.5grams (tonearest10 reg.)of the ground paper. Weigh at.thesame time,samples for moisture and ash de-terminations.

5.2 Immediately befcre use,add 5,0mill-ilitersof copper sulphatesoiutionto 95 mil-lilitersof carbonate-bicarbonate.solution.Bring the mixture to a boil in ?minutes, anilpour it aver 1.”5grams of the ground sampiein a 125-milliliter Erlenmeyer !Iask, Stirwell with a g!ass rod in order to distributethe fibers and to remove air bubbles. Fit theflask witina Icwselytittingghss bulb orst.cp-per and submerge ccmpieteiy in a steam bathat atmospheric pressure. Occaaionaily fiberstend to float to the surface, therefore the

should be shakenfrom tizne to time to. ,tribute them. F&move the thsk fromthe steam bathat the endof3 hours.Fi!teroilan ashlessfilterpaperina 7,5:entimeter13ucbnerfunnel,usingsuction.Wash byflooding with 100 milliliters cf 5 percentNa.,CO, solution at about 20” C. and then byflooding with 250 milliliters of hot water(about 95C C.), discarding the filtrates.Transfer the fibers and filter paper to a smallbeaker, add 25 milliliters of the molybdophos-phm-ic acid solution and macerate well witha flattened glass rod. Transfer to a Ettichnerfunnei again and wash thoroughly with coldwater until the blue molybdenum color is re-moved from the fibers. Dilute the filtratewith water to approximately 700 millilitersand titrate it with O.05 N KMnO, to a faintpink.

IJU-P-31b


Method 220

5.3 Thecopper number isthe number of fibrous materials. Correction of the weightgrams of metallic Cu in the CU,O resulting of the test specimen shall always be made forfrom the reduction of the CUSO. by ’100 moisture and ash. Not less than two deter-grams of thepaperfihers. This iscnlculated minations shall be made and tbe average ofby the formula: the results rounded off to the neareat 0.1,

6.36 x ml. KMnO. x Nshell be reported. Duplicate determinations

Copper number =should agree within 0.2.

w 6. Report

where N is the normality of the KMnO,, and 6.1 Thecopper number shall be reportedW is the weight in grams of the test speci- to one decimal place on the basis of totalmen after deduction of the weight of the non- fiber content.

UU-P-31b

II



MOISTURE \.

43

1. SUlpe

1.1 This method is for determining theamount of moisture in paper.

2. Test apecimene

2.I When the amount of moisture is de-termined to compute the results of chemicaltests of paper on a moistur’e-frse basis, thetest specimens shall weigh not less than 1gram and preferably not less than 2 gramseach, and when weighed shall be in moistureequilibrium with the specimens being ana-lyzed. When moisture is determined to com-pute the amount of moisture in a delivery ofpaper, the test specimens shall weigh notless than 50 grams each, and they shall beobtained in accordance with method 160. Insampling a delivery for moisture content, ex-treme care shall be taken to avoid change inmoisture content during sampling. Handlethe specimen with clean, dry rubber gloves,transfer it to the container as soon as with-drawn, and close the container immediately.If a delay of over a second or two in trans-ferring the specimen to the container is un-avoidable, keep the specimen covered on bothsides with several adjacent layers of the pa-per from which it was withdrawn until readyto place it in the container. Unless the speci-men is later to be spread out in the oven,avoid stuffing the container tightly.

3. Apparatus

3.1 The speciaI apparatus reqnired forthis test is an airtight container in which thetest specimen is dried and weighed. For theminimum size of specimen designated, aweighing bottle approximately 65 nrilli-meters (2% inches ) in height and 45 milli-meters (131* inches ) in diameter is suitable.For the larger specimens, a ProPOrtiOnate~Ylarger, lightweight, airtight metal can should

be used, preferably containing a removablelightweight wire-mesh basket.

3.2 The oven used to dry the paper sha!lbe equipped with means for ensuring ade-

quate temperature control and air circluiahic:iand preferably equipped with means of dry-ing the air entering the oven.

4. Procedure

4.1 After the specimen has been placedin a weighed container, weigh it in the closedcontainer to obtain tbe moist gross weightof the sample.

4.2 For large samples, unless the con-tainer has a removable basket, take the speci-men from the container in which they wereweighed, spread them in a basket or traywhich will permit free circulation of airaround them, and place them, as well as theoriginal containers, in the oven. Heat for

about 2 hours, replace the specimens in theoriginal container and close it, doing this ifpossible without removing the specimensfrom the oven. Let the closed container andcontents cool at room temperature, andweigh.

4A For small samples, without removingthe specimens from the weighing bottles, re-move the stoppers, heat. for 1 hour, close thebottles in the oven, cool to room temperaturein a desiccator, and weigh. Remove the stop-per momentarily just before weighing, toadjust any change in air pressure.

4.4 Dry the s~imens in either case at100” to 105” C. Repeat the periodical dryingand weighing until the difference in weightbetween two successive weighings is nOtmore than 0.1 percent of the weight of the

UCJ-P-31b


Method 240

specimen. For ‘2-gram samples, all weigh- 5. Reportings shallbemade toan accuracyof1 milli-gram; forethersamples.at]easttoan ~cCu- 5.1 Themristureshallbereportedastheracyof1/2000oftheorigimlweightoftine percentage!CSSintheoriginalweightofthesample. papertothel]earest0.1.

UU-P-31b



1. Scope

L 1 ‘This method is fm the qualitativeand quantitative determination of rosin(colophony) in paper.

2. Qualimtive tests

2.1 A pesitive result .abtaim?dby both ofthe following procedures shall be regardedas conclusive evidence of the presence ofrosin or rosin soap added as a sizing ma-terial.

2. L 1 Lic?imvrmn-.%orch tat. — P 1aceabout 1 gram! of the paper, cut into smallpieces, in a clean, dry test tube. Add 5 miHi-Mers of C.P. acetic anhyciridi and boil downto about 1 milliliter. (Cazaton--The fumesOf ihe anhy&jde are very irritating andshould be burned w they leave ike mouth ofthe test tube. ) Pour the liquid residue intoa clean, dry porcelain, :.wcible and coo) tomorn t.eiuperature m ;iawer, If any waxypal titles separate out, they should be filteredoff on a drj filter pap~r. Add carefully downthe side uf the crucible. 1 dro? of concen-trated suip.iuric acid. ;A fugitive, rmw-vioietcoloration formed where ~he acid meets theanhyd ride ir.dicates r.wn.

~.~.z ,~~$p~~ttq~~... .P~ace the paper on

a glas3 or ?mrcela?::;tateand apply a dropof a nexrly wt..;:a:(..!.+olutionof sugar. Aftera few w:.:*:, :s remove the excess sugar solu-tion .with fi!ter paper. Add a drop of concen-trated H, SO, to the sugar on the paper. Araspberry-red cokiraticn indicates the pres-ence of ros!~.

3. Quantitative determimtiim

3.1 Test specirrwn.-The test specimenshall consist of strips about 0.25 by 1.6inches (6 x 40 mm. ) weighing 5 to ‘7 grams.

3.2 Apparatus.-A suitable extractionaPParatu% such as a Soxhlet or Underwrit.

ers’, is required.

3.3 Extracting $otvent.–-To 1 liter of 95percent ethyl alcohoi add 4 milliliters of rxm-centratml HCI and mix.

3.4 PmccduTc.--Place the strips len@h-wise in the syphon cup of the extractor, taki-ng care to avoid packi~g them togethertightly. For tine extraction, we about 2 to2.6 times the vcJume of soh~ent required totill the syphon cup. Extract at a rate of 15syplwcings per hour (which should yield avolume of shout 250 ml. of solvent dis-tilled par hour) for a period of 2 honrs.

3,4.1 When the extraction period ;s com-pleted, avaporate off tbe sohent in the flaskon the steam bath until the odors uf alcohcland HCi are no longer noticeable. Place theflask ~i.an even ai 100° to l@5°C. for 15 min-utes, c~i to room temperature and add 20rnilliiitera of anhydrous ether. The rosin cii6-solves in from 5 to 30 secomis, but if co~>eredby foreign material it must be uncovered byscraping the mass with a stirring rod..4fter standing 15 to 20 minutes to furtherthe coagulation and settling out of the for-eign rmticr ifmzcessary,filtertheetherso-iution with suction through a fine-pore tilterpaper cut to tit a Gooch cmcible, directly intoa weighed beaker. It is usually necessary torefilter the filtered solutim through the samepaper. Another 20-milliliter portion of etheris used for rinsing, adding the rins; ng to thesolution in the weighed container. Evapo-rate the ether, then dry in an oven at 100’”to 105oC. for 15 minutes and weigh to thenearest 1 milligram. Repeat drying andweighing until tbe weight is constant to plusor minus 1 milligram.

3.5 Report.—The result of the rosin deter-mination shall be reported to the nearest 0.1as a percentage of the paper dried at 100° to106”C.

UU-P-31b


I

FIBER

1. scope

Method 3003 M4trci lW

IDENTIFICATION AND QUANTITATIVEDETERMINATION

1.1 This method covers the identificationof the kinds of fibers present in paper andpaperboard, and their quantitative estima-tion when the material contains mixtures ofdifferent kinds of fibers.

2. Teat specimen

2.1 The specimen for test shall consist,when possible, of pieces having a total areaof 25 square centimeters (4 sq. in.) cut fromdifferent portions of the test sample so as tobe representative of it. If sufficient specimenis not available, an area of 3 square centi-meters ( ~2 sq. in. ) will be recognized forquantitative analyais and 0.9 square centi-meter (1/s sq. in. ) for fiber identification.

3. Apparatus and materials

3.1 Microscope.-A compound microscopeequipped with a mechanical stage, Abbe con-denser, eyepiece, and achromatic objective. Amagnification of 100 diameters is recom-mended. This is obtained by using a 16-mili-meter objective and a 1O-X Huygenian eye-piece. If the microscope has an adjustabledraw tube, a 160-millimeter tube length isused; and if an apochromatic objective ieemployed, it is necessary to use a compensat-ing eyepiece and an achromatic condenser.

3.1.1 Counting eyepiece.—The eyepieceehall be equipped with a suitable referentspoint (cross hairs, pointer, or dot) forceunting the fibers passing under it.

3.2 DmPPer.-A glass tube 6 milli-meters in internal diameter and about 10centimeters long, fitted at one end with a rub-ber bulb and having tbe other end carefullysmoothed but not constricted. Tbe tube shallbe graduated at the lower end eo as to deliver0.5 cubic centimeter.

3.3 Slties and cover gfaeea.-slidei and

cover glasses shall be kept in 60 percent al-cohol, or washed with it before use. Theslides shall be 1 inch x 3 inchj of colorlessglass. The cover glass shall be 1 inch square(No. 2).

3.4 Hot pkzte.-The hot plate shall havea solid metal top with an absolutely level sur.face and be capable of heating to 50° to 60” C.The top of the hot plate maybe painted witha dull black paint, well baked-on, and thenmarked with suitable lines te correspondwith the lines on the ends of the slides. Thisis for convenience in making up aamplen.

3.5 Dissecting needlee.

3.6 Aluminum soap 8olution.

3.6.1 To 600 dubic centimeters of dis-tilled water add 15 grams of pure white soapshavings (Ivory soap is satisfactory) andstir until completely dissolved; then add 10grama of pure aluminum sulphate, Ali-(S0.) ,.18 H,O, and stir until the pr~ipi~taforms a wax-like mass of A1-atearate whichmay be Iifted out with a stirring md. Placethe precipitate in a desiccator for 48 houreor more. Store in a well stoppered bottle foruse es needed.

3.6.2 To 50 cubic centimeters of benzenein a glass-stoppered bottle add 0.7 gram ofthe A1-stearate and ahake well daily untilcompletely dissolved. This usually requiresabout 10 days.

3.6.3 If, after standing for severslweeka, the mixture should appear to havelost some of its water-repelling capacity, asmall piece of A1-stearate dropped into thesolution will wrrect this condition within afew hours.

A Disintegration of teet apecfmen

4.1 Tear the test epecimen intu smaflpieces and place in a small besker. Obtain

UU-P-31b


LMethod 300

the approxi!nate we!ght of the specimen in

order to calculr.tethe proper dilution of thedisintegrated specinren. Cover with l-per.

cent FJaOH solution,bring to a hoi! on a hoi

plate,decanttheliquid, and wash twice with

distil!edwater. Cover with (?.05,\rIf(.I:,letstand, Se>.er~lrylinu~eS,decant the acid, and

wash several tbrres with distilled water.I)rain ofi Lhe ‘water, rollthe piece:;of paperinto pelle~ gentty lretween the t!run!b ?r!d

fingers,put into a 500-milliliterErlenmeyerflask, adda little water and shakevigoimus!yuntil the water is absorbed by the paper.Add more water and shake, and continue thistreatment until the paper is thoroughly de-fiimru!, Di!ute the suspension of fibers bypouring away part of it and addinE water tothe remainder untii the suspension has a con-sistency of abo,ut 0.05 percent fibers. Pa.r-ti~l!y ii!i a test tube with. the mixture.

5 Preparation of slides-.

.5.1 Keep the microscope slides and coverglasses in 50 percent alcohol. After the slideshave been dried and polished, draw lines onthem 1 inch from each end in the following%.anner: Arrange si:* slides or less so thatthe ~dges am in contact. Place a 6-inchwooden rule [tl inc}! -wide and having a metalferru!e) on the slides sc that the rear eifgeof the rule is ewn with their snds. Dip aclean steel pen ill an ordiliary pe,l iloider~nto tile Al-soap solution, and let the excesstlc..v oti’ by touch; fig the point to the edge ofthe hOtt!e. Draw a line on the slides along

the metal edge cf the ruler. Repeat the op-eration cm tbe opposite ends of the slides.This gives a thin line of A1-stearate acrosseach slide 1 inch from each end, and these\ines wiil kwp the fiber suspension withinthe area of 1 square inch at each end of theNide. It is advisable to wipe the pen pointclean after each set of markings. Removedust and lint from the slides with a smallcamel-hair brush; then place the slides on thehotpiate at about 60” C. Thehot plate must

middie of the suspension and withdraw aportion of the mixture. P1ace 0.5 cubic cewtimetms of the suspension immediately oneach end of the slide. (’The test t~he must ●W shaken and sample withdrawn for eachend of the slide). Evaporate a portion ofthe water, then carefdly tap the suspensionwith a dissecting needle to distribute thefibers evenly inside the l-inch-sqtiare areason the end of each slide. Leave the slides onthe irot plate until completely dried. Theyare then ready for stsining as describedunder the various stairrs.

Nom 1,—.Caremust be taken that the unstainedfibersm tbe slifleare not touched by the maiys?ssn~iXS. ‘Theslideshould be allowedto coolb-efo?eadding the stain,otherwisecmfusing colorsmay beobtained.

6. Procedure

6.1 Examine the prepared slides micro-scopically, usiilg a magnification of about 100diameters. Yor a quantitative estimation,place tbe stained slide on the mechanical.stage of the microscope and count the differ-ent. kinds of fibers acrmst heslide, beginning2.5 millinreters from onekmgedgeand mak.ing five trips across one end of the slidealong lines spaced e.pproxi.mately 5 milii. ●meters apart. The distribution of fibers onthe slide shall be such that five trips acrosstbe slide at 5-millimeter intervals will in-clude between 200 and 300 fibers. Repeatthis on the sample on the other end of theslide. If these two results agree within 5percent, no further counts need be made;otherwise another count shall be made on oileend of a second slide and tbe three resultsaveraged.

6.1.1 As each fiber pasees under the ref-erence point in the eyepiece, count it as oneregardless of its size. If aggregations oftihers, such as occur in grotmdwood, are en-countered, tbe number of single fibers in theaggregation shall be egtimated and countedas if the fibers were separated completely.

be level.7. Stnining andidentitication

5.2 Thoroughly mixthetest-tuhe suspen-sion of the sample, insert the dropper tO the 7.1 Herzberg stain.

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Method 300

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7.1.1 .Preparethe followingsolutions:

(a) Anaquemmsolutionof C.P.zincchlo-ride (fused sticks in 50-grmn, unbroken,sealed bottles) saturated at 20° C.

(b) 0.2’5 gram of Cl’. iodine and 5.25grams of C.P. potassium iodide dissolved in12.5 cubic centirneterof distiiled water.Mix 25 cubic centimeters of solution (a),measured at 20° C., with solution (b). Pourinto a narrow cylinder and let stand untilclear (12 to 24 hours). Decant tinesuperna-tant liquid into an amber-colored glass-stnp-persd brittle and add a smal} piece of iodineto the solution. Avoid undue exposure tolight and air.

7.1.2 Forstainifig, apply 30r4 drops oftbe stain to the dried fibers, covertbe wholewith a coveii glass in such a rnmner as toavoid air hubbies, let stand for 1 or 2 min-utes, and drain off the surplus by tippingthe slide edgewise on u blotter,

7.1.3 The followink’colors are developedby this stain:

Red—Linen, cotton, ldeached rnanilahi?mp(abaci).

Blue-Chemically prepared fibers low inlignin, from wood, straw, and es-parto.

Yellow—Fibers high in lignin, such asgroundwood, (unbleached) jute,and unbleached manila hemp(abaci).

7.2 Lofton-MwriU stain. —This stainshall be limited to difierentiatim betweenconiferous (softwood) unbleached sulphiteand coniferous (softwood) unbleached sul-phate.

7.2.1 Prepare the fnllowing solutions:

(a) 2gramsof malachite green in100cu-bic centimeters of water.

(h) 1 gram of basic fuchsin in 100 cubiccentimeters of water.

Mix these in the proportion of 1 part ofsolution (a) to2 parts of solution (b). Adda few drops of the compound stain to thefibers and let stand 2 minutes, Remove ex-

cess stain by means of a hard filter paperand add a few drops of 0.1 percent HCI,.4fter about 30 seconds remove tbe excessacid. Finally add a few drops of water andremove the excess.

7.2.2 As dyes frcm difierent sourcesvary, it is necessary to test them by stainingknown fibers. Llnbleached sulphate fibers arestained blue or b!ue-green and unbieachwlsulphite fibers puxple m !awmder. If anypurple fibers appear in unbleached suiphatefibers, this in.dicatesthereiston much fuch-sin present and more malachite green solu-tion must be tiddsd. The opposite is indi-

cated if some unbleached sulphite fibers de-

velop a green or blue color.

7,3 Modified Brigkt stain. —This stainshall Ibe used onhy tn show’ t~kepresence ofgrmindwocid and unbleached Iwlps. Pewent-ages of unbleached or groundwood pulp

found by this metinodmay belOwrtha~l theactual arncunt present, due to the factthaisonw vjell-m[ked unbleached pulp may failto give a blue color.

7.3.1. Prepme the following solutions:

(a) 2.7 grains of ferric chl,oride, FeCl,f3H,,0,pm jOO cubic centimeters of distilledwater.

(b) 3.29 grams ofpotassium ferricyanide,K,Fe(CN),, per 100 cubic centimeters of dis-tilled water.

(c) 011 grams of benxopurpurin 4B crudein 100 cubic centimeters of 50 percent ethylalcohol. The dye used shall be DuPont Pur-purin 4B Concentrated, or its equivalent. Thesolution is warmed until the dye is complete-ly dissolved. (Some of the dye will precipi-tate nn cooling. )

Filter solutions (a) and (b) and keep inseparate bottles. These solutions should berenewed frequently. Solution (c) may beused indefinitely. When the solution be-comes cloudy, warm until it becomes clearagain.

7.3.2 Apply 3 dropa each of solutions(a) and (b) to’the fibers and let stand 1minute. Remove the excess stain by means

UU-P-3 lb


Method 300

of blotting or filter paper, add a few dropsof solution (c), and let stand 2 minutes.Finally remove water, using a glass cover.

7.3.3 Any blue coloration of fibers showsthe presence of groundwood and/or un-bleached pulps. Bleached fibers or fiberspractically free from ligno-celhdose stainred.

8. Calculation of results of quantitativeestimation

8.1 Multiply the number of each Kind offiber counted by ite factor as given in tableI to obtain the weighted count. Add togetherthe weighted counts of each kind of fiber andcalculate each to a percentage of the total.

Table I.—Weight factors for diflerentkinds of fibers

E

Groundwwd ----------------------Line”andcotton------------------Chemicalconiferouswood----------Chemicsldeciduouswood----------

9. Report

9.1 The proportions of the various fibersfound shall be reported in terms of percent-ages by weight of the total fiber compositionto tbe nearest multiple of 5. When any fiberis found present in amount less than 2VZper-cent, it shall be reported as “trace.”

9.2 In reporting results by the Herzbergstain the following nomenclature shall beused:

Rag (cotton, linen, hemp) ......EspartoConiferous chemical wood .......Jute or manilaDeciduoue chemical wood .......StrawMechanical wood ......................Japanese fiber

When stains other than the Herzberg areused, appropriate qualifying terms may beapplied, such as bleached, unbleached, eul-phate, sulphite, etc.

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I Copiesof this specificationmaybs purchasedfor.2Scents.

I

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wJ.S.GOVERNMENT PRINTINGOFFIGS:1971.714-15’V12C’16

UU-P-31b


INSTRUCTIONS: In ● -ntin.ing ●ffoti 10 nuke our .ta.dardiz.tion documenk belter, the 00D Prnridn fhts form for w in,

..bnutting comments and sussatioN for immvc=n~. All uwx Of mili~w *~nd~r~l=tiOn *-* ~ **N k ~wsuggestions. lliii form IMY be daschrd, folded ●tone the tin- indicated, taped slow the 1- edge (DO IVOT STAPLE), MCItikd. In block S, tw n opccitic u pamibte ●bout putic.kr problem ueu such u wordins which mqttktwd iat.?rptw-tioa, wu

too risid. mctrictite, IOMC, ambisuotu. or wu incompatible, and give proposed wordiw chansa which wotdd d.tetitethe

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aptcification rrquiremrnts on current contrmb. Comments submitled cm this form do not cmwtitute or itaply .uthodutionk, wmivr ●ny portion of the refem.ced document(s) or to amend contract.at requirements.

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