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    TC A623

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    ASTM 623

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    TC A623

    Copyright:

    © All Rights Reserved
    Download as PDF or read online from Scribd
    Flag for inappropriate content
    42 views16 pages

    Astm 623

    Uploaded by

    ledaswan
    TC A623

    Copyright:

    © All Rights Reserved
    Download as PDF or read online from Scribd
    Flag for inappropriate content
    of 16
    AG A 623m - 06 the tn erystal pattern. The size ofthe tin crystals is estimated by comparison with ASTM macro-grain size number stan- dards. A33. Apparatus (Required Only for Method No. 3) A331 Polarized Light Source and Analyzer © ‘ABA Reagents and Materials (Required Only for Method. No.) A34.1 Purity of Reagents—Reagent grade chemicals shall bbe used in all ests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the ‘Committee on Analytical Reagents of the American Chemical Society, where such specifications are available Other grades may be used, provided itis first ascertained that the reagent is of sufficiently high purty to permit its use without lessening the accuracy of the determination. ‘A3.A2 Purity of Water—Unless otherwise indicated, refer fences 10 water shall be understood to mean distilled water or water of equal pity. ‘A343 Cotton or Soft Cloth A344 Ferric Chloride (FeCly6H,0)—Chemically pare rade ‘A3.4.5 Hydrochloric Acid (HCI) (IN)—Chemicaly pare rade ‘A346 Sodium Sulfide (NagS:9H,0) or Sodium Bisulfate (NaH1SO,H,0)—Chemically pure grade ABS Test Specimen ‘A3.5.1 The sample consists of any convenient size piece of fused electrolytic tin plate 25.8 cm?or larger. A36 Procedure ‘A3.6.1 Method No, 1—Fertic chloride etch. ‘A36.1:1 Prepare etching solution by dissolving 100 g of FeCly-6 HO and | g of Na,S-9 H,0 or NaHSO,-H,0 in 1000 mL of 1 NV HCl. Solution is reusable but should be replaced when etching of specimen takes longer than 30 s. ‘A3.6.1.2 Bulf surface of specimen vigorously but with ight pressure with cotton or soft cloth. This disrupts the passive film nd permits the etching solution to attack the tin readily. ‘A3.6.1.3 As an alternative to A3.6.1.2 and, ifthe equipment is available, cathodically clean specimen in 0,5 % sodium carbonate (Na,CO,) solution for 30's. Reversing the polarity of the current for J 5 aear the beginning of the cleaning cycle assists fa removal of the passive layer. Rinse in tap water. A36.1.4 Immerse specimen in etching solution for 5 to 15 sor until a crystal pattern develops, Remove, rinse in tap water, and dry. (Do not allow the specimen to remain in the etching solution too long as complete detinning will occur) ‘A3.6.1.5 Estimate the tin erystal size number by comparing the specimen with ASTM macro-grain size number standards (Gee Test Methods E 112.) For routine testing, itis convenient touse a set of secondary standards consisting of actual cn plate specimens or photographs thereof at } X magnification, ‘3.62 Method No. 2—Iron solution value disk, A3.6.2.1 Examine the specimen after completion of the ISV fest (See Annex Ad) as it will already be suitably etched, ‘A3.6.2.2 Estimate tin crystal size same as in Method No. 1 ‘A3.6.3 Method No, 3—Polarized light. A3.6.3.1 This is a rapid nondestructive method. ‘A3.6.3.2 Place the specimen in a beam of polarized light so the beam strikes the surface obliquely ‘A3.6.3.3 Examine the reflected light beam through an ana- Iyzet. Rotate the analyzer to obtain best definition of tin crystal patter. A3.6.34 Estinfate ! elpiga RST And Harber Oe, West Cestohocken, Fema 1526258, ‘A4. METHOD FOR DETERMINATION OF IRON SOLUTION VALUI INTRODUCTION It is not intended that variations in apparatus, sample preparatibal described in this standard method be precluded. Suppliers or consumers may employ such variations for control purposes provided results agree with [AA.L Scope ‘A4L.1 The iron solution test also called the ISV text, is cone of four special propeny tests used to measure cenain characteristics of electrolytic tin plate which affect intemal corrosion resistance. The test i applicable to. nominal tin coating Weights 5.62.8 g/m, and heavier electrolytic tin plate (for Keplate, ee 3.1.13.2 and Fplate, see 3.1.13.1). Its not applicable © 28/28 and lighter electrolytic tin plate |A42 Summary of Method ‘A42.1 The iron solution test involves the colorimetric determination ofthe total arpount of iron dissolved when 20°3 ‘cm? of tin plate surface area are exposed for 2 h at 27 + 0.5°C to 30 mL of @ mixture of dilute sulfuric acid (HS), (H,0;), and ammonium thiocyanate from ASTH Internationa those obtained by the standard method, (NH,SCN). The amount of iron dissolved expressed as micro- ‘grams is arbitrarily called the iron solution value (ISV). Ad3 Apparatus® A43.1 Cabinet, Room, or Other Means of mai +£ 0.S°C during the test run. 4.3.2 Test Vessels, ound, tall-form, wide-mouth, approxi- ‘mately 236-mL glass bottles with 63-mm diameter plastic caps, ‘A4.3.3 Gaskets made from 1.59-mm thick vinyl sheeting. Gaskets have Si-mm inside diameter (ID) and 61.5-mm outside diameter (OD). ‘A434 Burets—Two 25-mL automatic filling rapid dispens- ing burets. ‘A4.3.5 Equipment for Cathodically Cleaning Test ‘Specimens—The power source should be capable of supplying ining 27 PELE MAR ca, This copy has been made ty the iret for Sanat and Quay (TAMER) under Herse 1 to 16 A pet test specimen (26-cm? disk). A stale beaker or tank is recomimended as the cleaning vessel as it may also serve as the anode. ‘A436 Spectrophotometer and Cuvettes. ‘A44 Reagents and Matertals ‘A44.1 Purity of Reagents—Reagent grade chemicals shal be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specificstons of the Commitee on Analytical Reagents of the American Chemical Society, where such specifications are available.* Other grades, ‘may be used, provided itis fist ascertained that the reagent is Of suliiently high purity to permit its use without lessening the accuracy of the determination. ‘84.4.2 Purity of Water—Unless otherwise indicated, refer ences to water shall be understood to mean distilled water or water of equal purty ‘A443 For Cleaning Test Specimen: ‘A443.1 Acetone. ‘8443.2 Sodium Carbonate Solution (Na;CO,) (05 %). ‘A444 For Iron Solution Test ‘44.4.1 Ammonium Thioeyanate Solution (Iron-Free) (NHSCN), ‘A442 Hydrogen Peroxide Solution (H,0,) (30 %). ‘A4A43 Sulfuric Acid (H,S0,) 2.18 N) ‘AMA For Calibration: ‘A445.1 Tron Wire, Analytical ‘A445. Sulfuric Acid (H;S0,) (10 ¥). AAS Procedure AGS. Test Solutions: A4S.1.1 Prepare a3 % solution of H,O, by dilution ofthe 30% grade. ‘A45.12 Prepare acid-peroxide stock solution by mixing in following proportions: 23 mL of H,S0,(2.18 N) to 2 mL of H0,( ). (This mixture remains stable for several weeks.) Connect acid-peroxide stock solution bottle 10 one of the 25.miL automatic filling rapid-dispensing bures. ‘A45.1.3 Prepare a stock solution of NH,SCN (40 g/L.) and connect the stock botle to the other burt ‘A452 Sample Preparation: ‘8452.1 The specimen consists ofa fat-circular piece of tin plate $7.33 * 0.03 mm in diameter. This is equivalent to 25.8, cem®. The specimen must be typical ofthe plat bein tested and free of incidental deep scratches and surface conditions that are not representative ofthe tin plate under tes ‘A4 52.2 Cathoically clean the specimen in 0.5% Na,CO, solution for 30 s. Near the beginning of the cleaning cycle reverse the potaity of the current for I's This 1-s anodic ash assists in removal ofthe oxides on the surface. ‘A45.23 Rinse the specimen successively in tap water and Aistlled or deionized water, Dry in acetone vapors. Do not touch the test surface ‘A453 Iron Solution Test ‘A45.3.1 Place the cleaned specimen, test surface up, in the plastic cap. (Paper liner should previously have been removed. To facilitate seating of gasket, the last 1.59 mm of cap thread may be removed by machining on @ lathe.) Copyright STH Inert 10 Bar Habre, West Conshohecken,Penesyvania. 19428-2859, SRESESSE nts lates of aera, Ts cp has ben made » the trate fox Strand Quay (TAME) unde ices the specimen, seating it so that the gasket lies flat and holds the specimen firmly in place. ‘A4.5.3.3 Add 25 mL of the HSO,-H,0, stock solution and 25 mL of the NHSCN solution to the test vessel. Swirl to assure thorough mixing. A4S.34 Alix the cap with specimen and gasket tothe test vessel. Secure tightly. Invert the vessel immediately and let stand for 2'h at 27°C without agitation or vibration. ‘A45.3.5 Provide one extra test vessel for each run. Add 25 mL each of the two stock solutions, cover with a plastic cap, ‘but do not invert. This mixture will act as a blank during the calculation of the iron solution value. ‘A45.3.6 After 2h, swirl the liquid once, turn the vessel upright, and remove cap, gasket, and specimen immediately. Repeat for all test vessels in the run. Remove cap from the blank. (Warning—A small amount of hydrogen cyanide gas ‘may be liberated during test run. Be sure the vessels are opened in a well-ventilated room or preferably under a hood) A4S.3.7 Add 1 mL of 3% H,O, to each test vessel including the blank. Add the peroxide just before transferring the liquid in each test vessel zo the cuvette. (See A4.8) ‘A4.5.3.8 Set the spectrophotometer at 485 nm, Zero the instrument by setting the scale for 100% transmission on disifed or deionized water. ‘A45.39 Transfer a portion of the liquid to a cuvette and record the optical density or percent transmission, depending ‘on the original calibration. If the instrument has been fited with an ISV scale, read the /SV directly ‘A4S53.10 Rinse the vessels successively with tap water and distilled or deionized water as soon after test as possible, Quick rinsing minimizes the buildup ofa yellow sulfur deposit, Periodically the vessels should be cleaned with sulfuric acid- dichromate cleaning solution to remove the deposit, ‘A4S.3.11 Soak gaskets fora few minutes in dilute H,S0,, rinse with distilled or deionized water and hang on a glass rod tw dry. (Heating the H,S0, to around 66°C during the soaking Of the gaskets assists in removal of any iron compounds and helps retain resiliency of the gaskets.) ‘A46 Calibration ‘A46.1 The spectrophotometer and cuvettes should be cali- brated with standard solutions containing known amounts of iron. A typical calibration might proceed as follows: ‘A4.6.1.1 Prepare standard iron solution by dissolving 0.100 1g of iron wire in 100 mL. of 10 NV HySO.. Dilute with distilled Water to 1000 mL. in a volumetric flask ‘46.1.2 Using aliquots, also prepare 10+1 and 190+1 dilutions of this solution. These three will give standard iron solutions containing 0.1, 0.01, and 0.001 mg Fe/mL, respec- tively ‘A4.6.13 Mix 25 mL of the H,S0,-H,0, and 25 mL of the NH,SCN stock solutions as in A4.5.3.3. Add I mL of the standard iron solution containing 0.1 mg Fe/mL. Repeat using the 0.01 and 0,001 mg Fe/mL. standard iron solutions. The three ‘mixtures will give iron solution values (/SV) of £00, 10, and 1, respectively. 4.6.1.4 Measure the optical densities at a wavelength of 485 nm in a spectrophotometer and plot these against the /SV's. A a chink for Standards and Quality (STAMEQ) under license "frum AST nai Optical 1 10 ‘The /SV is ditectly proportional (o optical density. A typical calibration curve using a Coleman Model 6A Junior spectto- photometer” * and 19 by 150-mm round cuvettes is shown in Fig. A4L. A fuil logarithmic plot is used o enhance the definition x the low end of the ISV scale where most readings ‘occur, Once the calibration is established the simplest proce- dure is to make and attach a scale to the spectrophotometer which reads directly in /SV. ‘A&T Calculation 'A4.7.1 If the spectrophotometer does not have an JSV scale, determine the SV from the calibration curve for each sample including the blank. ‘A4.7.2 Subtract the blank ISV from each of the scale SV readings or from the [SV's oblained in A4.7.1. This isthe true sv. AGB Interferences A481 Leakers—Sometimes leaks will occur. These are ‘generally discovered when the vessels are opened atthe end of the test. Ifa leak has occurred, a local spot of iron-tin alloy or bare steel will show near the edge of the specimen or ctching, Aiby ‘Copyright ASTH Ielesalianal 100 Bar Harbor Drie, Auliy ox Conshohocken, Pennsyvania 13428-2858, APL (pte Sates of Americ. Tis copy has been made 1000 Isv FIG, A4.1 Tplea! Iron Solution Value Calbration Curve R ‘may be seen on the reverse side of the disk, or both. Sometimes the leak will not affect the /SV; at other times it may cause an extremely high ISV. Any test showing a leak or other irregu- larity should be discarded and a retest made. ‘A482 Detinning or etching of the tin plate disk by any ‘other cause than the normal exposure tothe reagents may cause erroneously high results. Such detinning or etching could be ‘caused by, (J) inadvertent too long anodic flash or 100 long ‘exposure to Na,CO, in sample preparation (see A4.5.2.1), (2) agitation, swirling, or vibration of test vessel during 2-h test time, (3) leakers, and (4) rise in temperature. ‘A48.3 Fading of the red ferric thiocyanate complex color may occur due to decomposition of the complex by excess peroxide. Delay between the adding of the peroxide at the end. of the test and the reading of the optical density should be avoided. Also care should be exercised not to add more than the I mL of peroxide, A49 Precision ‘A49.1 The principal source of error in reproducibility of test results is variation in the tin plate itself. Variation may ‘scour across the rolling width and along different portions of the same coil of tin plate. Generally plate with low ISV has ‘uch less variation than plate with high ISV. Plate Lots B, D, E, and F as follows show the type of variation that can occur 4G} A 62am - 06 when replicates of a given plate lot with all specimens closely adjacent to each other are run at one time. Plate Lots A and C show the type of variation that can occur when replicates of a given plate lot ae run singly in tests over a long period of time, ron Sokon Value, mg on 2 6 2542 se ® z o rs es . F 7 roe ‘e « 35035 samples in range rom 81012 ‘A492 Is reommended theta least oe specimen from 2 Pate ot age ange das amber of n we evaten ‘Songee fot of plate 8 4 oe 1 6 svc io os beater De, é u woes nO 7 ch, =< 188-05, AS. METHOD FOR ALLOY-TIN COUPLE TEST FOR E INTRODUCTION ‘The method described in this specification for conducting the alloy-tin couple ext is one of several possible methods to obtain the same test result Iti no intended thal other methods or variants ofthis Inethod be precluded, Variation in apparatus, reagents, test media, and procedure from those specified may be employed for control purposes by the consumer or the supplier provided satisfactory results Are oblained which correlate with the specified method, ASA Scope AS33 Magnetic Stirrer AS.L.1. The alloy-tin couple test,!® also called the ATC test, is one of four special property tests used to measure certain characteristics of electrolytic tin plate which affect internal corrosion resistance. The test is applicable to nominal tin coating weights 5.6/2.8 gim? and heavier electrolytic tin plate (Gor K-plate, see 3.1.13.2). [vis not applicable to 2.8/2.8 p/m? and lighter electrolytic tin plate AS2 Summary of Method ‘AS.2.1 The ATC testis an electrochemical procedure which involves measuring the current flowing between a pure tin electrode and an electrode consisting of a piece of tin plate from which the free (unalloyed) tin has been removed to expose the iron-tin alloy, The measurement is made after 20-h exposure of the electrodes in a medium consisting essentially of deaerated aged grapefruit juice. ASS Apparatus ‘AS3.1 Constant-Temperature Cabinet or Room (27 + 05°C), ‘AS32 Test Cell (Fig, AS.1): AS.3.2.1 Borosilicate Glass Test Cell, approxi capacity. ‘AS3.22 Poly(Methyl Methacrylate) Plastic Cover for test cell approximately 12:7 mm thick drilled with 15.9-mm diameter holes to accommodate cell elements. ‘A5.3.2.3 Polychloroprene or Similar Synthetic Rubber O-Ring Gasket to effect seal between glass vessel and plastic ‘cover or equivalent method to effect gas-tight seal 53.24 Silicone Rubber 6.35-mm Thick Grommets to act as gas-tight holders for cell elements inserted through the plastic cover, ely 1.5L "Kamm. GG. Wiley. AR Bees RE. and KrikJ Ly “Corosion Rexsaace of Elevolyte Tin Pte, Part 3 Te Ay-Ti Compe Testa New Research Took” Coron, ot 17,161 p84, 3 A534 Low-Resistance, High-Sensitivity Galvanometer!® ‘AS3.5 Potentiometer to measure the tin electrode potential. ‘Any high-impedance voltage-measuring device such as a pH eter with a O to 1300-mY scale is satisfactory. ‘45.3.6 Calomel Reference Electrode (Bither saturated or 0.1 Nis satisfactory). A537 Power Source capable of supplying variable de voltage for use in sample preparation (cathodic cleaning 10-V dde and tin stripping 0.4-V de reducible to 0.2 V). ‘A5.3.8 Various Elecirical Components such as plugs, jacks, switches, and resistors to permit construction of circuit de- Picted in schematic diagram (Fig. AS. ‘A5.39 (Optional) Special Die for applying microcrystalline Wax to mask off known areas on test specimen.* ® AS Reagents and Materials AS4.1 Purity of Reagents—Reagent grade chemicals shall be used in all ests. Unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available.* Other grades ‘may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination, ‘A342 Purity of Water—Unless otherwise indicated, refer ences to water shall be understood to mean distilled water or ‘water of equal purity. ‘AS43 Test Medium: ‘A3.43.1 Distilled Water or Deionized Water of equal purty AS.4.3.2 Ethanol, Denatured (10 % volume). AS.43.3 Frozen Concentrated Grapefruit Juice. A54.34 Nitrogen Gas (High-Purity Oxygen-Free Dry Tank Nitrogen). "A Leeds ne Nortup Mode 2430, 25.0 glvanomee i 003 pre sensi or alent has en Gand sats "in Ghactrede Thermometer apg ASTM Iteration, 100 Bar Harr Die, West Conshobacken, emsyfaris 1548-2958, ie Stats of Ameca Ths copy has been made FIG. AS.4 Toat Col! Used in tho ATC Tost AS435 Potassium Sorbate ‘5.4.3.6 Pure Tin Wire (approximately 3.18-mm diameter), ‘5.4.3.7 Sodium Hydroxide Solution (NaOH) (10 %). ‘45.438 Stannous Chloride Solution (SoCly2 H,0), A544 Sample Preparation: ASAI Acetone, A54.4.2 Microcrystalline Wax (140 to 145°F melting point). ‘AS4.43 Poly(Methyl Methacrylate) Plastic Strips 1.59 by 143 by 82.6 mm. ‘AS4.44 Sodium Carbonate Solution (Na,COs) (0-5 %. ‘AS4.4.5 Sodium Hydroxide Solution (NaOH) (5 %. ASS Test Specimen AS.5.1 The specimen consists ofa piece of tin plate cut 12.7, bby 114.3 mm wit the long dimension transverse to the rolling direction. ‘A5.5.2 Eight test specimens can be accommodated at one time in the apparatus described above. Only the number of specimens to be included in one run should be prepared at one time. 4 4ST International. AS.S.3 Details of sample preparation are given in AS.7. ‘AS.6 Preparation of Apparatus (Fig. AS.2) A561 Drill 15.9-mm diameter holes in 12.7-mm thick plastic cover to accommodate eight test specimens, the pure tin anode, a thermometer, and cooling coil. The reference elec- ‘rode bridge can be inserted through one of the test specimen ‘openings during potential measurement. Dill smaller diameter holes into the cover to accommodate ges inlet and outlet tubes ‘A5.6.2 Cut stoppers or grommets from 6,35-mm. thick silicone rubber to fit snugly in 15.9-mm diameter openings. Cut holes or slits in stoppers and grommets to hold various cell elements. Boil all rubber parts including O-ring gasket in 10 % NaOH solution for S min and rinse thorough!y Before use in distilled or deionized water. ‘45.6.3 Thoroughly clean test cell and its components and finally rinse them in ethanol just prior to use to guard against ‘mold and yeast growth in test medium. 'A5.644 Fit silicone rubber parts, cooling coil thermometer, and gas tubes into the cover. Do not insert pure tin anode or test specimens at this time. Aly A 623m - 06 LOO boon. 6.x itn ASIN Intemational, Phone Jack Copyright ASTA International, 100 Bar Harbor Die, West Conshohocken, Pennsyvania 19428-2958, of America, This copy has been made an Quality (STAMEQ) under license [Pig [potentiometer FIG. A5.2 Schematic Diagr AS.6.5 Form 3.18-mm diameter pure tin wire into a loosely wound coil to give a total surface area of approximately 100 ‘em?, Cathodically clean in 0,5 % Na;CO, solution, rinse in tap water and in acetone. AST Procedure ‘ASIA Test Medium: ‘AS.ZL.I Place a polytetraftuoroethylene-covered magnetic stirring bar inthe bottom of the test cell. ‘AS7.12 In a separate vessel, dilute frozen concentrated grapefit juice 3+1 with dislled or deionized water, add preservative potassium sorbate to give concentration of 0.5 B/L, deaerte by heating to boiling, and transfer tothe tet cell and age for not less than two days. Leave approximately {6.35.mm headspace. Tur on the magnetic stirrer. ‘ASZL3 Assemble the plastic cover tothe test ceff with an (O-ring oF by other leak-proof sea, Begin the flow of nitrogen through the headspace. Bubble nitrogen through distilled or deionized water before entering the test cell in order to minimize evaporation of test medium. Maintaia a slight pos tive pressure in the cell during actual test run by bubbling nitrogen from the gas outlet tube through 25.4 or $08 mm of ‘water oF 12.7 mm of dibutyl phthalate ‘AS.1.14 Allow the transferred bot juice to cool for 5 min; then start cold water through the cooling coil. This minimizes setling of the pulp. Continue cooling until the test medium reaches 27°C. 'AS.Z.1.5 Insert the cleaned pure tn anode into the test cell. AS.6 Add SpCly2H,0 to produce a concentration of 0.190 g/L. This yields a Sn** concentration of 100 ppm. Continue stirring for Sor 10 min to make sure the SnCly2H,0 has been dissolved. ‘AS.T-L1 Discontinue siing Somale Yin Electrode 1 of ATC Test Ciroult AS.7.1.8 Measure the potential of the tin electrode with a high-impedance device such as a pH meter, using calomel reference electrode. The potential of the tin anode should be 615 mV against a saturated calomel electrode or ~105 mV against a 0.1 N calomel electrode. ‘A512 Test Specimen: ‘AS7.2.1 Degrease the specimen in acetone and allow to dry ‘AS7.2.2 Clean the specimen cathodically in 0.5 % Na,COy solution (carbon anode) using a current density of approxi- mately 25 mA/em?, A 10-V de power source with a polarity reversing switch and the following sequence of test specimen polarity is suggested: 2 s cathodic, 0.1 s anodic, 2 s eathodic, O.1 s anodic, 2 s cathodic. The wo short anodic flash treatments enhance the ability of the cathodic treatments t0 remove oxides and impurities from the surface and secure absence of water break on the test specimen. Rinse the specimen in ap water, distilled water, and acetone and allow to ‘A5.1.2.3 Detin the specimen electrolytically in aS 9 NaOH. solution at room temperature. The specimen isthe anode and piece of stainless steel is the cathode, The area of the stainless Steel cathode should be 5 to 10 times as large as the area being = weight of extracted oil, mg, and A_ = area of sample, em ‘To convert to gySITA: divide mg/m? by 10. AG Precision and Bias AG.I1.1 Make all weighings to the nearest 0.0001 g. METHOD B—DETERMINATION OF TOTAL ‘SURFACE OIL ON TIN MILL PRODUCTS BY ELLIPSOMETRY ‘AG.12 Scope ‘A6.12.1 This method covers the determination of the total oil on the surface of tin mill products by ellipsometry. AG.13 Summary of Method ‘A6.13.1 The basic ellipsometer is a highly accurate optical instrument that measures the change in the polarization state, referred to as the ellipticity, of light reflected from a surface. ‘The change in ellipticity before and after degreasing is the ‘measured variable and related to the oil layer thickness. AG.14 Apparatus ‘A6.L4.I Ellipsometers measure the change in polarization state of light reflected from a surface and provide information about the optical properties of thin films on that surface. Certain ellipsometers are specially designed for measurement of oils on tin mill products." * Ellipsometers not specifically Aesigned for measuring oils on tin mil oils could be calibrated to measure tin mill oils; however, that is beyond the scope of this method. ; ‘AG.15 Reagents and Materials AG.15.1 Non-residue forming degy Trichloroethylene or I-Bromopropane. A616 Hazards AGI6.1 Trichloroethylene and 1-Bromopopane vapors present a potential health hazard. An exhaust hood js required for operation of the ellipsometer. ing solvent such as AG.17 Preparation of Apparatus AG.I7.1 Itis necessary to set up the instruments’ various gain and sensitivity adjustments for different substrate surfaces (for example, varying brightness or tinplate versus TFS), Once set up is achieved for a sample type, the settings can be recorded and used for future testing of the same sample type, Set up does not affect calibration, but instead, adjusts measure- ‘ment circuitry for best overall performance. Newer models Teste sore of supply ofthe appara known the commie sis tie ‘s Donat Elecones, le, #0. Bot 27 MeDonad PA 1507 q Zama td lates of America THs Copy hasbeen made Directorate for Standards and Quay (STAMEQ) under license Mibrmaaae 06 sstomcally adj these stings. The following se FO dure for oker models sithout the automatic adjustment hes been found to provide the best epeataiiy, ands provided se example ‘86179 ‘The instrument has a High Volage Power Suply Control ected above the Operator Control Pane. Tis contol is marked 5 ~ 10. Each full sting (5 ~ 10) is X 100, For example: 5» SOOV with setting x 50 Example 55 = S50 ‘ACh tine the muller should be st to "0". The Panel Meter shout ead "0 Se the Reading switch to Base (46173 nl atypia spl of the type to be measured wit the rong dteton in the vet! potion. (A617 Set high voltage contol to 5O0V. Set the NULL control to "10" clockwise: Set the MULTIPLIER Control to “I% The pane! Meter should have moved someplace above o 'AG7S Tam high voltage UP jst until ful scale meter deflection is cheered on the Patel Meter Note the High Volage ting and add 1S0V ~ 250V forthe final vokage sting For ekampl: Fl meter defection SSOV. Final sting is 550 + 250 or 00V. Even though the meters past fl sal, itis protected by intemal erutry. This ithe comes meter position forthe begining or afte the nd of acct. the Ra oliage sting eed to be higher than TOODV, the Milter Control shoul e reset higher, and then repeat setup. "A617 Pus stan button (Leave moor switch off) Use the inch sieht jog the Amp Mtr needle down unt it sare coming back p."This should be near 10 microamps. Tur the NULL conol counterclockwise unl the needle reads be: Oween = 5 microamps, ‘86177 Turn the motor switch on, The ellipometer will fish running its cyte. Tum the Clean Switch of. St the Reading Switch to OIL. Press the Manta! Stat But. You should etx reading between 9.98 and 002. The lipsometer ts now st up. AS long asthe needle defection fs within the parameters of <10 to 90 >, no changes are necessary. No justmens aro be made afte the nit is setup, unless the Surface of the prodvt changes AG.18 Procedure ‘A6.18.1 Samples for oil weight determinations are obtained by stamping disks 5733 + 0.02 mm in diameter, whichis, equivalent 25.81 cm? per side. Copyrih AST Iteration 100 Bare Hrhor Drive, West Conshohocken, Pennsylvania 15428-2958, ‘AE.1&2 Samples should be handied on the edges and free of seratches, fingerprints and other contaminants. A sample that has been dmpped or touched on the surface should be discarded. ‘A6.18.3 Insert the sample into the magnetic sample holder the rolling direction in the vertical position. ‘A6.18.6 Verify that the Null control, Multiplier, and High Voltage settings are set up correctly as described in A6.17. ‘A6.18.5 Set the Reading Switch on the Operator Control Panel to the Oil position. ‘A6.18.6 Set the Clean Auto/OMT Switch to the Auto position. ‘6.18.7 Depress the Manual Start bution to initiate the ‘measurement. At the completion of the measurement and cleaning cycles the oil weight can be read directly from the digital display in grams/base box. ‘A6.188 IF the opposite side of the sample isto be measured rotate the sample and repeat step in A6,18.7. Itis advisable that fone side per sample is measured to prevent spray-over to the ‘opposite side during the cleaning cycle. ‘46.189 If significant time is to pass between procurement and testing, 2 sufficiently large shect should be cut and sandwiched between two coversheets and sealed with tape to prevent oil evaporation. The test samples can then be stamped from the sheet prior to testing. 6.18.10 The in-factory calibration of the ellipsometer (degrees of analyzer rotation/unit of oil weight per surface area is for melted (reflowed) tinplate with a bright stone finish. It is the responsibility of the instrument user to develop a ‘correction factor for different coatings, or finishes, or both, as needed or as agreed upon by manufacturer and purchaser A6.19 Precision and Bias A6.19.1 Four laboratories measured the repeatability using different coil for each laboratory. The standard error was 0.25 mg/m? for 30 samples with oil Weights ranging from 5.0 to 12.5 mplm?. A reproducibility study could not be conducted due to volatilization of the oil ‘A6.19.2 The in-factory calibration of the ellipsometer (de- agrees of analyzer rotation/unit of oil weight per surface area Lunt) is for melted (reflowed) tinplate with a bright stone finish. I is the responsibility of the instrument user to develop a correction factor for different coatings, oF finishes, or both, as needed or as agreed upon by manufacturer and purchaser. A7. DETERMINATION OF CHROMIUM ON TIN PLATE BY THE DIPHENYLCARBAZIDE METHOD. ATL Scope AT.L-1 This method! covers the determination of chro- ‘mium on tin plate with the use of diphenylcarbazide. A72 Reagents A721 Purity of Reagenis—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended Furman, NH, “Chromium in Aci Solon wit pelea,” Soa" Sendont Mets of Choma Anal, Vo 1, 1962. pe 337-3. that all reagents shall conform (0 the specifications of the ‘Committee on Analyticai Reagents of the American Chemical Society, where such specifications are available.” Other grades ‘may be used, provided it is first ascertained thatthe reagent is Of stficiently high purty to permit its use without lessening the accuracy ofthe determination ‘81.22 Purity of Water—Unless otherwise indicate, refer ences 19 water shall be understood to mean distilled water or water of equal purty A123 Chromaie, Standard Soluion A (I mL = 0.5 mg Cx)—Dissolve 1.410 g of K,Cr,0, in water and dilte to 1.0L. Sy the Directorate for Standards and Quay (STE) nde ese sep eration — 06 A124 Chromate, Standard Solution B (I mL = 10.0 yg ‘C)—Pipet 20 mL of the chromate Standard Solution A into a LO-L volumetric ask and add water to 1.0 L. ‘A725 Diphenylcarbazide Reagent—Add 10.0 mL of ac- tone, 10.0 mL of 95% ethyl alcohol, and 20.0 mL of H,PO,(85 % acid diluted with an equal volume of water ‘A126 Hydrochloric Acid (HCD) (sp ar 1-19) ‘A127 Potassium Permanganate Satarated Solution (KMn0.). A128 Sodium Hydroxide (1.0 N}—Trisodium Phosphate (5%) Solusion—Dissolve 40.0 g of NaOH and 50.0 g of [Ne,PO, in water and dilute to 1.0 L. A129 Sulfuric Acid (143)—Add 100 mL of H;SO,(sp er 1.84) slowly and with stiring to 300 mL. of water. ‘A73 Procedure A7.1 Use for analysis sample having 52 em* of surface ae (one 26-em* disk. If both sides of the sample are to be Stripped, slighty bend the disk through the centers it will not Tie entirely flat. Ifonly one sie ofthe sample is tobe stripped, hold the disk tightly against a rubber stopper. The stopper shouldbe sight larger in diameter than the disk and grooved toallow vacuum from a tube inthe center to be applied to most ofthe surface ofthe disk. Leave intact a band approximately 3.2 mm wide atthe perimeter ofthe stopper. 'A73.2 Place the sample i « 250-ml. beaker, ald 25 mL of NaOH.Na,PO, solution, and heat to boiling. Boll for 1% min. “Transfer the solution to another 250-ml. beaker, washing disk and beaker once with water Add 25 ml of H,SO,(1+3) to the ‘original beaker and sample, heat to boiling, and boil 1 min. “Transfer the acid solution to the beaker containing the alkaline stripping solution, washing sample and beaker with two small portions of wate If both sides ofthe disk are being stripped, itis necessary 0 switl the beaker continually over the flame while the H,SO, is boiling. This is necessary to keep the surface completly wetted and strip all ofthe chromium from the surface of the tn plate ‘A133 Heat the sample solution to boiling and add 1 to 2

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