Preparing and Evaluating Specimens For Automatic Inclusion Assessment of Steel

 

 

Designation: E768  −  99 (Reapproved 2010)

Standard Guide for

Preparing and Evaluating Specimens for Automatic Inclusion Assessment of Steel1 This standard is issued under the fixed designation E768; the number immediately following the designation indicates the year of  original adoption or, in the case of revis original revision, ion, the year of last revision. revision. A number in paren parenthese thesess indicates the year of last reappr reapproval. oval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Sco Scope pe 1.1 Thi Thiss gui guide de2 cover coverss two preparation preparation method methodss for steel metallographic specimens that will be analyzed for nonmetallic inclusions inclusi ons with automa automatic tic image analysis (AIA) equip equipment. ment. Thee two me Th meth thod odss of pr prep epar arati ation on ar aree of offe fere red d as ac acce cept pted ed methods meth ods use used d to ret retain ain non nonmeta metallic llic inc inclus lusion ionss in stee steel. l. Thi Thiss guide does not limit the user to these methods. 1.2 A pr 1.2 proc oced edur uree to te test st th thee su suita itabi bilit lity y of th thee pr prep epar ared ed specimen for AIA inclusion work, using differential interference contrast (DIC), is presented. 1.3 1. 3 Th Thee va valu lues es sta stated ted in SI un units its are to be re rega gard rded ed as standard. No other units of measurement are included in this standard. 2. Referenc Referenced ed Documents Documents 2.1   ASTM Standards:3 E3 Guide E3  Guide for Preparation of Metallographic Specimens E7   Terminology Relating to Metallography E7 E45 Te E45  Test st Method Methodss for Determining Determining the Inclusion Content of  Steel E883   Guide for Reflected–Light Photomicrography E883 E1122 P E1122  Prac ractice tice for Obt Obtain aining ing JK Inc Inclus lusion ion Rati Ratings ngs Usi Using ng 4 Automatic Image Analysis (Withdrawn Analysis  (Withdrawn 2006) E1245   Prac E1245 Practice tice for Det Determ ermini ining ng the Inc Inclus lusion ion or Sec Second ond-Phase Constituent Constituent Conten Contentt of Metals by Automatic Automatic Image Analysis

1

This guide is under the jurisdiction of ASTM Committee E04 Committee E04 on  on Metallography and is the direct respon responsibil sibility ity of Subco Subcommitte mmitteee  E04.01  E04.01   on Specimen Preparation. Current Curre nt editio edition n appro approved ved Nov Nov.. 1, 2010. Published Published Janua January ry 201 2011. 1. Origin Originally ally approved in 1999. Last previous edition approved in 2005 as E768–99(2005). DOI: 10.1520/E0768-99R10. 2 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:E04-1002. 3 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [email protected]. For  Annual Book of ASTM  Standards volume information, refer to the standard’s Document Summary page on the ASTM website. 4 The last app approve roved d vers version ion of this historica historicall sta standa ndard rd is refe referenc renced ed on www.astm.org.

2.2   ASTM Adjuncts:5 ADJE0768 Differential Interference Contrast Magnification 100X and 500X (6 micrographs) 3. Terminology 3.1   Definitions: 3.1.1 3.1 .1 For definition definitionss use used d in thi thiss pra practic ctice, e, ref refer er to Term ermiinology   E7 nology E7.. 3.1.2   differential interference contrast microscopy— a comprehensive definition appears in Guide E883 Guide  E883,,  paragraph 11.8. 3.2  Definitions of Terms Specific to This Standard: 3.2.1   rigid rigid gri grindi nding ng dis disk—  k— a non non-fa -fabri bricc sup suppor portt sur surfac face, e, such su ch as a co comp mpos osite ite of me meta tal/c l/cer erami amicc or me metal tal/p /pol olym ymer er,, char ch arge ged d wi with th an ab abra rasi sive ve (u (usu suall ally y 6 to 15 15-µ -µm m di diamo amond nd particles), and used as the fine grinding operation in a metallographic preparation procedure. 4. Signi Significanc ficancee and Use 4.1 Inclusion ratings done either manually using Test Methods   E45  or automatically using Practice   E1122  ods E1122   or or E1245  E1245   are influenced by the quality of specimen preparation. This guide provides prov ides examp examples les of prov proven en specime specimen n prepar preparation ation methods that retain inclusions in polished steel specimens. 4.2 This gui guide de pro provid vides es a pro proced cedure ure to det determ ermine ine if the prepared prepar ed spe specime cimens ns are of sui suitab table le qua quality lity for sub subseq sequen uentt rating of inclusions. None of these methods should be construed as defining or establishing specific procedures or limits of acceptability for any steel grade. 5. Preparat Preparation ion Methods 5.1   Background: 5.1.1 5.1 .1 The inclusio inclusions ns in the plane of pol polish ish must be ful fully ly preserved and clearly visible. Preparation should not produce excess exc essive ive reli relief ef aro around und the per perimet imeter er of the inc inclus lusion ionss tha thatt would wou ld exa exagge ggerat ratee the size and number number of inc inclus lusion ionss on the 5

A colored plate, consisting consisting of six micrographs micrographs that illus illustrate trate the use of DIC in determining a prope determining properly rly prepared sample (at 100x and 500x), is available from ASTM Headquarters. Order Adjuct:  ADJE0768  ADJE0768..

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E768 − 99 (2010) TABLE 1 Comparison of ANSI (CAMI) versus FEPA versus Median Diameter of Grit Size in Micrometers

plane of polish. In many cases, the preparation of specimens forr in fo incl clus usio ion n ra ratin ting g is mo more re re read adily ily pe perf rfor orme med d af afte terr th thee specime spe cimens ns hav havee bee been n har harden dened ed by a sui suitabl tablee hea heatt tre treatme atment nt procedure proced ure (auste (austenize, nize, quench to fully martensitic structure, temper at a relatively low temperature). 5.1.2 Cleanlin Cleanliness ess is an impor important tant consideration consideration in all stages of specimen preparation. 5.1.2.1 5.1.2 .1 Heat-tr Heat-treated eated specimens should be wire brushed or shot blasted or have the surface ground to remove adherent scale. 5.1.2. 5.1 .2.2 2 After com comple pleting ting the gri grindi nding ng ste steps ps and bef before ore performing the polishing steps, the specimens and specimen holders must be cleaned to prevent contamination of the next preparation step. Cleaning the specimens and specimen holders between betw een each gri grindi nding ng step can elim elimina inate te con contami taminat nation ion of  coarse abrasives to the following finer preparation step. 5.1.2.3 5.1.2 .3 After the preparation preparation is complete, swab the surface carefully with cotton and a water/soap solution containing a corrosion inhibitor such as a machine coolant or ethyl alcohol solu so lutio tion n to re remo move ve an any y film filmss or ot othe herr de debr bris is th that at wo woul uld d interfere with the inclusion rating. 5.1.2.4 5.1.2 .4 It is advis advisable able to perform the inclusion analysis analysis as soon as possible after preparation to minimize staining or other problems that can affect the analysis. 5.1.3 5.1 .3 The two met method hodss tha thatt fol follow low have been found found to be reliable procedures for retaining inclusions in steel and achieving the desired results when evaluated by DIC. There are other methods that will result in a quality specimen as revealed by DIC. Each laboratory should develop preparation procedures forr th fo their eir ma mater teria ials ls so th that at th thee pr prep epar ared ed su surf rface acess me meet et th thee requirements requir ements prese presented nted in in   6  of this guide. 5.1.4 As described described in Prract Prractice ice   E3 E3,,   the specimens may be sectioned and mounted to ease handling during preparation. It is advisable to use a mounting medium that is hard enough to preserve edges and maintain flatness. 5.1. 5. 1.5 5 Abras Abrasiv ivee gr grit it si size ze de desig signa natio tions ns in th this is gu guid idee ar aree expressed expres sed in the Americ American an National Standards Institute Institute (ANSI) or Coated Abrasives Manufacturers Institute (CAMI) system units with the corresponding Federation of European Abrasive Procedure (FEPA) numbers in parentheses. Table parentheses.  Table 1 provides 1  provides a correlation correl ation between these two systems and the approximate approximate median particle diameter for a given grit size in micrometres. 5.1.6 Most preparation preparation systems systems apply pressure on the specimens being processed. The best pressure to be used for each preparation step should be determined experimentally. Conversions between applied force and pressure are discussed in the Appendix X1. X1. NOTE  1—Care must be taken to protect the polished specimen surface from scratches or contaminants when using a specimen leveling device.

5.2   Silicon Carbide Procedure: 5.2.1 5.2 .1 A summary summary of the sili silicon con carbide carbide pro proced cedure ure can be found in Table in  Table 2. 2. 5.2.2 When using a semi-au semi-automatic tomatic polishing polishing equip equipment, ment, grinding grind ing and polish polishing ing should be perfo performed rmed using appro approxiximately 18 kPa pressure per specimen. (For a specimen holder containing six 32-mm mounts, a force of approximately 87 N must be applied (see X1.4.2 (see  X1.4.2). ).

ANSIA (CAMI)B 

FEPAC 

Approximate Median Diameter (µm)

60 80 100 120 150 180 220 240

P60 P80 P100 P120 P150 P180 P220 P240 P280 P320 P360 P400 P500 P600 P800 P1000 P1200 P2400 P4000D 

250 180 150 125 90 75 63 58.5 52.2 46.2 40.5 35.0 30.2 25.8 21.8 18.3 15.3 8.4 3.0

280 320 360 400 500 600 800 1200 A

ANSI - American National Standards Institute CAMI - Coated Abrasives Manufacturers Institute C  FEPA - Federation of European Abrasive Producers D  Not a FEPA designation B 

5.2.2. 5.2. 2.1 1 Low pr pres essu sure ress ar aree re reco comm mmen ende ded d to en ensu sure re th thee retention of an assortment of inclusion types found in a variety of steel grades. The relatively low pressures suggested in this procedure will not necessarily result in a satisfactory polish for etching and the further evaluation of the specimen’s general microstructure. The pressures used in the following rigid disk  procedure are more likely to result in a surface more satisfactory for reveali revealing ng gener general al micros microstructu tructures. res. 5.2.3 5.2 .3 Gri Grind nd the spe specim cimens ens on ANSI 80 gri gritt (P8 (P80 0 FEP FEPA) A) silicon sili con car carbid bidee pap paper er to ens ensure ure all sect section ioning ing art artifa ifacts cts and deformation damage have been removed and the entire specimen surface is co-planar to the grinding surface. NOTE  2—If the sectioning method resulted in a smooth face and little deformation damage, and if after securing the specimens in a fixture for polishing, the entire surface of interest is co-planar to the grinding surface, then finer grit papers, such as ANSI 180 to 240 (P180 to P240 FEPA) can be used for the initial grinding step.

5.2.3.1 An adequate 5.2.3.1 adequate flow of water should remove all loosened abrasive and grinding debris from the paper during the grin gr indi ding ng pr proc oced edur ure. e. Th Thee flo flow w of wa wate terr sh shou ould ld en ensu sure re th thee specimen is kept cool during grinding. 5.2.4 5.2 .4 Con Continu tinuee gri grindi nding ng thr throug ough h the seq sequen uence ce of sili silicon con carbide papers listed in  Table 2. 2. It may be necessary to clean the samples between every grinding step to prevent contamination of the next preparation step. 5.2.5 After completing completing the entire grinding grinding operation, operation, clean the specimens thoroughly, using ethyl alcohol and cotton, then rinse and dry. Ultrasonic cleaning can be used. 5.2.5.1 5.2.5 .1 The use of a soap and water solution in an ultrasonic ultrasonic cleaner can attack non-metallic inclusions in some carbon and low alloy steels, leading to an exaggeration in the inclusion’s appare app arent nt size size.. Adding Adding an inh inhibit ibitor or (su (such ch as tha thatt use used d as a machining coolant) may reduce this size exaggeration.

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E768 − 99 (2010) TABLE 2 Prepara Preparation tion Method I Silicon Carbide Carbide Abrasive Paper Grindi Grinding ng

Surface

Coolent/   Lubricant

Abrasive Size/Type ANSIA [FEPA]B 

Paper

Water

80 [P80] grit SIC

Paper Paper Paper Paper Paper Paper

Water Water Water Water Water Water

120 [P120] grit SIC 240 [P240] grit SIC 320 [P500] grit SIC 400 [P600] grit SIC 600 [P1200] grit SIC 800[P2400] grit SIC

NAP free cloth

Extending fluid

3 µm diamond

Low nap cloth

Extending fluid

1 µm diamond

Low nap cloth

Extending fluid

1 µm diamond

Time (seconds) Planar Grinding 60 Fine Grinding 60 60 60 60 60 Rough Polishing 50 Final Polishing 50 Optional Polishing (manual) 50

ForceC  newtons [lbs]

Surface Speed RPM

Relative Rotation

14 [2]

300

ComplementaryD 

14 14 14 14 14 14

[2] [2] [2] [2] [2] [2]

300 300 300 300 300 300

Complementary Complementary Complimentary Complementary Complimentary Complementary

14 [2]

150

Complementary

14 [2]

150

Complementary

relatively high

NA

NAE 

A

American National Standards Institute (ANSI) designation of grit size. Federation of European Producers of Abrasives (FEPA) designation of grit size. C  Force per 3-mm (1.25-in.) diameter specimen. specimen. D  Complementar Comple mentary y rotati rotation, on, surface and specimens spin in same direction. E  Since this optional step is completed manually, manually, these two catego categories ries are not applicable. applicable. B 

5.2.6 Polish the specimens specimens using 3-µm diamond diamond abrasive abrasive on a low nap cloth, such as woven wool, for 50 s. Clean and dry the specimens as described in 5.2.5 in  5.2.5.. 5.2.7 Polish the specimens specimens using a 1-µm diamond diamond abrasive on a high nap cloth for 50 s. Clean and dry the specimens as described in 5.2.5 in  5.2.5.. 5.2.8 5.2 .8 A final man manual ual polishing polishing step may be add added, ed, using 0.25-µm diamond abrasive on a low nap cloth for 10 to 20 s, using relatively high pressure. Clean and dry the specimens as described in 5.2.5 in  5.2.5.. 5.2.8. 5.2 .8.1 1 Ultr Ultraso asonic nic clea cleanin ning g is not rec recomm ommend ended ed aft after er the final manual or automatic polishing step. Ultrasonic cleaning can cause cavitation damage, ultimately distorting the inclusion sizes. NOTE 3—Depending on the material, it may be advisable to avoid water after polishing.

5.3   Rigid Grinding Disk Procedure:

5.3.1 A summar summary y of the rigid grinding grinding disk disk procedure procedure can be found in Table in  Table 3. 3. 5.3.2 Semi-a Semi-automati utomaticc grind grinding ing equipment is requir required, ed, with specimens contained in a circular fixture for the entire procedure. For 5.3.2-5.3.5 For  5.3.2-5.3.5,,   a pressure of 42 kPa should be applied per specimen. (For a specimen holder containing six 32-mm circu cir cular lar mo moun unts ts,, a fo forc rcee of ap appr prox oxima imatel tely y 20 203 3 N mu must st be applied applie d (see (see X1.4.3  X1.4.3). ). 5.3. 5. 3.3 3 Gr Grin ind d fo forr at le leas astt 15 s af after ter ac achi hiev evin ing g a co co-p -pla lana narr condition, using a 150-grit alumina grinding stone at 1450 rpm or 80-grit (P80 FEPA) alumina/zirconia grinding paper at 300 rpm. 5.3.3.1 5.3.3 .1 An adequate adequate flow of water should remove all loosened abrasive and grinding debris from the paper during the grin gr indi ding ng pr proc oced edur ure. e. Th Thee flo flow w of wa wate terr sh shou ould ld en ensu sure re th thee specimen is kept cool during grinding.

TABLE 3 Prepar Preparation ation Method II - Rigid Grinding Grinding Disk Procedure Coolant/   Lubricant

Abrasive Size/Type ANSIA Ti Time me - se seco cond nds s [FEPA]B 

Alumina/zirconia paper

Water

80 [P80] grit

Alumina grinding stone

Water

Rigid grinding disk

Alcohol/glycol

Napless or stiff napped cloth

Alcohol/glycol

Soft short napped cloth

Alcohol/glycol

Porous Synthetic Cloth

Water

Surface

Planar Grinding >15 Or 150 [P150] grit >15 Fine Grinding 9 µm diamond 180 Rough Polishing 3 µm diamond 240 Final Polishing 1 µm diamond 120 Optional Polishing Alkaline Colloidal Silica or 90 Acidic Colloidal AluminaE 

Force Forc eC  newtons [lbs]

Surface Speed RPM

Relative Rotation

34 [8]

300

ComplementaryD 

34 [8]

1450

Complementary

34 [8]

150

Complementary

34 [8]

150

Complementary

34 [8]

150

Complementary

100 [23]

150

Complementary

A

American National Standards Institute (ANSI) designation of grit size. Federation of European Producers of Abrasives (FEPA) designation of grit size. C  Force per 32-mm (1.25-in.) diameter specimen. D  Complementar Comple mentary y rotati rotation on surfac surface, e, and specimens spin in same direction. E  Water is substituted for the colloidal oxide during the last 20 s. B 

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E768 − 99 (2010)

5.3.3. .3.2 2 It may be nec necess essary ary to clea clean n the samples samples between between 5.3 ever ev ery y gr grin indi ding ng st step ep to pr prev even entt co cont ntam amin inati ation on of th thee ne next xt preparation step. 5.3.4 Finish grind using using 9-µm diamond on a rigid grinding grinding disk for 3 m at 150 rpm, using an alcohol/glycol lubricant. Clean the specimens and fixture thoroughly (ultrasonic cleaning is helpful) with alcohol and cotton, then dry with forced air. 5.3.4.1 5.3.4 .1 The use of a soap and water solution solution in an ultrasonic ultrasonic cleaner can attack non-metallic inclusions in some carbon and low alloy steels, leading to an exaggeration in the inclusion’s appa ap pare rent nt siz size. e. Ad Addi ding ng an in inhi hibi bito torr (s (suc uch h as th that at us used ed as a machining coolant) may reduce this size exaggeration. 5.3.5 Rough polish polish using 3-µm diamond on a napless cloth (silk or non-woven chemotextile) or a low nap cloth (woven wool) woo l) for 4 min at 150 rpm usi using ng alco alcohol hol/gly /glycol col lub lubrica ricant. nt. Clean as in  5.3.4  5.3.4.. 5.3.6 Final polish using using 1-µm diamond diamond on a high nap cloth for 2 min at 150 rpm, using alcohol/glycol lubricant. Clean as in 5.3.4 in  5.3.4.. 5.3.6. 5.3 .6.1 1 Ultr Ultraso asonic nic clea cleanin ning g is not rec recomm ommend ended ed aft after er the final polishing step. Ultrasonic cleaning can cause cavitation damage, ultimately distorting the inclusion sizes. 5.3.7 5.3 .7 An opt option ional al oxi oxidede-pol polish ishing ing step step,, usi using ng a por porous ous synthetic cloth with either alkaline colloidal silica or acidic colloidal alumina, may be used if necessary to eliminate fine scratches. The conditions are 90 s at 150 rpm, 100 N, with water substituted for the colloidal oxide during the last 20 s. Clean as in  5.3.4  5.3.4.. 6. DIC Evaluatio Evaluation n Method5 6.1 A microscope microscope equipped equipped with DIC illumin illumination ation at magnific ni ficati ation onss of ab abou outt 10 100x 0x an and d 50 500x 0x sh shou ould ld be us used ed wh while ile developing the preparation procedure to verify the true surface topography topog raphy of prop properly erly prepared specimens. The sensiti sensitive ve tint

condition, using a first order gypsum (1 l) plate, is the most useful mode of DIC illumination (plane areas magenta; inclusions dark). 6.2 Ob 6.2 Obse serv rvati ation on at 10 100x 0x wi will ll re reve veal al wh whet ethe herr re resi sidu dual al scratches are present and whether background relief is evident. 6.3 At 500x in the DIC sensitive sensitive tint conditio condition, n, all of the edges of inclusion particles should be sharp and recognizable as sharp edges. Narrow bright lines indicating narrow ditches at some inclusion inclusion edges may, may, however, however, still be seen. A test may be made to determine whether these ditches will be detected by the image analysis system. 6.3.1 The polarizer polarizer is slowly rotated rotated away from the full DIC position positi on and the inclusion edges watched for apparent motion. There could be a critical trough configuration beyond which the bright troughs turn black at some point in the transition to bright field illumination, and the inclusions appear to become larger larg er.. This condi condition tion indica indicates tes insuf insuffficient prepa preparation ration.. (The use of a filar eyepiece eyepiece may be helpful at this point to determine whether the inclusion through has widened) 6.3.2 6.3 .2 Nar Narrow row troughs troughs can be acc accepte epted d as har harmle mless ss if the they y vanish van ish int into o the bac backgr kgroun ound d whe when n the pol polariz arizer er is ope opened ned a small part of its range. 6.4 Some fine scratches scratches from final polishing will usually usually be seen se en un unde derr DI DIC C at 50 500x 0x.. Th These ese no norm rmal ally ly als also o va vani nish sh on opening the polarizer and, therefore, should not affect quantitative measurement at lower magnification. NOTE   4—While 4—While hig highly hly ins instru tructiv ctive, e, the DIC exa examin minati ation on rem remain ainss subjective subjec tive with res respec pectt to the que questi stion on of whe whethe therr a rep reprod roduci ucible ble and accurate accura te surfa surface ce prepar preparation ation has been obtained. Tests Tests by actual measurement are necessary to determine that errors in specimen preparation were not contributory to outlier observations.

7. Keywo Keywords rds 7.1 automa automatic tic image analysis; differenti differential al interf interference erence contrast; inclusions; specimen preparation; steel

APPENDIX (Nonmandatory Information) X1. APPLIED LOAD CONVERSIONS CONVERSIONS

X1.1 Automatic prepar preparation ation machin machines es commo commonly nly displa display y applied force in either pound-force (lbf) or newtons (N). The ability to convert from one unit to another may be necessary when trying to interpret a documented procedure. X1.1.1 To convert from pound-force pound-force to newton, multiply the pound-force value by 4.5. X1.1.2 To convert from newton to pound-force, multiply the newton value by 0.225. X1.2 Whe X1.2 When n mul multipl tiplee spe specime cimens ns are held in a hol holder der,, the applied force must be divided by the number of specimens in the holder to determine the load per specimen. Some automated machines apply the load individually to each specimen

and display the applied load accordingly. X1.3 Cau X1.3 Cautio tion n sho should uld be tak taken en whe when n usi using ng aut automa omated ted machines chi nes tha thatt dis displa play y pre pressu ssure re in pou poundnd-for force ce per squ square are inc inch h (psi). (ps i). Typi ypicall cally y, the mach machine ine is dis displa playin ying g the air pre pressu ssure re within the loading cylinder cylinder and not the true pressure pressure applied to either the specimen holder or each individual specimen. X1.4 When X1.4 When co conv nver ertin ting g fr from om a fo forc rcee to a pr pres essu sure re,, th thee surface area of the specimen must be determined. The value of  forc fo rcee is th then en di divi vide ded d by th thee co cont ntact act ar area ea to de dete term rmin inee th thee required pressure. X1.4.1   Example 1— What What is the force in pound-force if 87 N is applied?

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E768 − 99 (2010) ~ 87 N ! 3 ~ 0.225! 5 19.6 lbf 

 

(X1.1)

X1.4.2   Example 2— What W hat is the applied load, in newtons, requ re quir ired ed to ap appl ply y a pr pres essu sure re of 18 kP kPaa to an in indi divi vidu dual al specimen in a holder containing six 32-mm circular mounts? Pressure = (Force)/(Area), therefore . . . Force = (Pressure) × (Area) Area =   P   r2 =   P  (16)2 = 804.25 mm2 Total Area = (6 mounts) × (804.25 mm 2) = 4825.5 mm2 18 kPa = 18 000 Pa = 18 000 N/m2 = 0.018 N/mm2 Therefore, Force = (0.018 N/mm2) × 4825.5 mm2) = 86.9 N

X1.4.3   Example 3— What W hat is the applied load, in newtons, required to apply a pressure of kPa to an individual specimen in a holder containing six 32-mm mounts? Pressure = (Force)/(Area), therefore . . . Force = (Pressure) × (Area) Area =   P  r 2 =   P  (16)2 = 804.25 mm2 Total Area = (6 mounts) × (804.25 mm 2 = 4825.5 mm2 42 kPa = 42 000 Pa = 42 000 N/m 2 = 0.042 N/mm2 Therefore, Force = (0.042 N/mm2) × 4825.5 mm2) = 203 N

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