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HPL/CSE/TECH/SE/4.4.4/01/03/OHPV confidential Gel Analysis of Polyolefin Film A. GEL COUNT OF LLDPE & PP FILM 1. Scope: This test method covers the determination of the number of gels present in LLDPE & PP films when observing the images formed on a screen when light is projected through the film. 2. Summary: The test methods encompass magnification of the film specimen by 7:1 (Method followed at ARDC) or 10:1 (Method followed at QA), thus making the images of the gels projected on a clean screen easy to see. Standard Sizing Template (suitably magnified) for determination of the size of gels and is employed. The defects so counted are classified according to their sizes and are reported as number of defects per square metre. Gels are believed to be composed of oxidized or high molecular weight materials, which is not readily blended into the polymer matrix. Surface defects arising out of poor blendability of additives may also contribute to gel like appearance. 3. Safety: Standard laboratory safety procedures are to be followed. The bright light of the overhead projector should not be directly looked at. 4. Interference:  Use of non-standard test equipment will limit the reproducibility between laboratories.  Contamination in the sample.  Inadequate purging of the extruder during processing of the film  Cross-contamination of the extruder during processing of the film  Contamination, scratches and marks in the film caused by poor handling  Contamination in the inspection apparatus from inadequate cleaning (dirty lens etc.)  Improper focus of the inspection apparatus  Excess magnification of the film specimen  Non-representative sampling (Incorrect sampling point, incorrect time of sampling) 5. Apparatus:  Film Properties Standard overhead projector: 2000 lumen capability 21 HPL/CSE/TECH/SE/4.4.4/01/03/OHPV confidential  Standard film mover  Standard wall chart viewing and sizing surface, approx. 1 gm x 2.0m., in size of heavyweight paper with matte finish with low gloss printing ink has sizing reference lines and circles for 0.1mm, 0.2mm, 0.5mm, 0.7mm. and 1.5mm sized for 10 times / 7 times magnification / projection of film.  Standard sizing Template Clear polyester OHP film template with sizing reference lines (parallel line separated by distances equal to 7 times or 10 times 0.1mm, 0.2mm, 0.7mm & 1.5mm) for use with the standard wall chart.  Coin – with about 25mm (1 inch) diameter. Alternatively clear polyester OHP film with a 1cm long line drawn on it using a marker can be used.  Vernier Calipers for accurate measurement of calibration coin accurate to 0.1mm.  Meter Ruler  Measuring tape  Clean soft cleaning cloths  Hand Tools 6. Test Method: Setting Up the Apparatus – Method Followed at QA  Set up the overhead projector and mount it on a table facing a clean white screen  Measure the diameter of the calibration coin precisely to the nearest 0.1mm with the vernier caliper  Multiply this dia. By 10  Turn on the projector bulb  Place the coin on the projector to project an image on the wall chart  Focus the projector so that the shadow of the coin edges appears as a sharp circle on the wall chart  Measure the diameter of the circle accurately with a metal ruler or measuring tape. This value should be within ±1% of the calculated in the step above  Move the table projector and film mover backwards away from or forward towards the wall chart until a 10x magnification of the coin is obtained Setting Up the Apparatus – Method Followed at ARDC  Set up the overhead projector and mount it on a table facing a clean white screen  Turn on the projector bulb.  Place the clear polyester OHP film with a 1cm long line drawn on it on the projector to project an image on the wall chart  Focus the projector so that a sharp shadow of the line appears on the screen  Measure the length of the image accurately with a metal ruler or measuring tape Film Properties 22 HPL/CSE/TECH/SE/4.4.4/01/03/OHPV  confidential Adjust the position of the projector till a 7X magnification of the 1cm long line is obtained. Test Specimens - LLDPE: A total film test area of 1520 sq.cm (240 sq. in) is employed for the testing, the area being divided into six specimens of 40 sq.in (8” X 5”) each. The LLDPE film samples shall be prepared by blown film extrusion and shall be of thickness 25±5 microns. Test Specimens – PP: A total film test area of 1520 sq.cm (240 sq. in) is employed for the testing, the area being divided into six specimens of 40 sq.in (8” X 5”) each. The PP film samples shall be prepared by cast film process (R103, F103) or tubular quench process (F110) and shall be of thickness 20±5 microns. Procedure:  Mark out an area of 8”X5” on each film specimen using a marker.  Place the film on the projector and view its image on the screen.  Circle the gels on the film using a fine tip marker.  Ascertain the size of the gels by placing the standard sizing template on each surface defect image projected on the screen. The size of the gel is taken as that closely matching a given reference line on the template.  Record the number of gels, classified according to their size for each test specimen.  Depending on specifications requirements, defects sizes may be 0.2mm – 0.49mm, 0.5mm – 0.69mm, 0.7mm – 1.5mm and >1.5mm. 7.Reporting: The report should consist the following details:  Complete identification of the material tested, formulation, lot number & date of manufacture.  Date of testing.  Date of film production & processing conditions.  Thickness of the film.  Number of film defects in each size category.  LLDPE: Number of defects per square meter in size categories – 0.2 – 0.5mm, 0.5 – 0.7mm & 0.7 – 1.5mm.  PP: The gel count is reported as per the table below: Gel Size category (0.2 – 0.5) mm (0.5 – 1.5) mm Test Method Number / 1520 cm2 ASTM D 3351 8. References:  MA 17108 Film Properties 23 HPL/CSE/TECH/SE/4.4.4/01/03/OHPV  MA 17329  ASTM D 3351 confidential B. GEL COUNT OF HDPE (MITSUI) FILM 1. Scope: This test method covers the determination of the number of gels present in an HDPE film when observing the images formed on a screen when light is projected through the film. 2. Summary: The test methods encompass magnification of the film specimen by 7:1 (Method followed at ARDC) or 10:1 (Method followed at QA), thus making the images of the gels projected on a clean screen easy to see. Standard Sizing Template (suitably magnified) for determination of the size of gels and is employed. The defects so counted are classified according to their sizes. Gels are believed to be composed of oxidized or high molecular weight materials, which is not readily blended into the polymer matrix. Surface defects arising out of poor blendability of additives are to be taken into consideration too. 3. Safety: Standard laboratory safety procedures are to be followed. The bright light of the overhead projector should not be directly looked at. 4. Interference:  Use of non-standard test equipment will limit the reproducibility between laboratories.  Contamination in the sample.  Inadequate purging of the extruder during processing of the film  Cross-contamination of the extruder during processing of the film  Contamination, scratches and marks in the film caused by poor handling  Contamination in the inspection apparatus from inadequate cleaning (dirty lens etc.)  Improper focus of the inspection apparatus  Excess magnification of the film specimen  Non-representative sampling (Incorrect sampling point, incorrect time of sampling) 5. Apparatus:  Standard overhead projector: 2000 lumen capability  Standard film mover  Standard wall chart viewing and sizing surface, approx. 1 gm x 2.0m, in size of heavyweight paper with matte finish with low gloss printing ink has sizing reference lines Film Properties 24 HPL/CSE/TECH/SE/4.4.4/01/03/OHPV confidential and circles for 0.1mm, 0.2mm, 0.5mm, 0.7mm and 1.5mm sized for 10 times / projection of film.  Standard sizing Template Clear polyester OHP film template with sizing reference lines (parallel line separated by distances equal to 7 times or 10 times 0.1mm, 0.2mm, 0.7mm & 1.5mm) for use with the standard wall chart.  Coin – with about 25mm (1 inch) diameter. Alternatively clear polyester OHP film with a 1cm long line drawn on it using a marker can be used.  Vernier Calipers for accurate measurement of calibration coin accurate to 0.1mm.  Meter Ruler  Meter ruler or measuring tape.  Clean soft cleaning cloths  Hand Tools 6. Test Method: Setting Up the Apparatus – Method Followed at QA  Set up the overhead projector and mount it on a table facing a clean white screen  Measure the diameter of the calibration coin precisely to the nearest 0.1mm with the vernier caliper  Multiply this dia. by 10  Turn on the projector bulb  Place the coin on the projector to project an image on the wall chart  Focus the projector so that the shadow of the coin edges appears as a sharp circle on the wall chart  Measure the diameter of the circle accurately with a metal ruler or measuring tape. This value should be within ±1% of the calculated in the step above  Move the table projector and film mover backwards away from or forward towards the wall chart until a 10x magnification of the coin is obtained Setting Up the Apparatus – Method Followed at ARDC  Set up the overhead projector and mount it on a table facing a clean white screen  Turn on the projector bulb.  Place the clear polyester OHP film with a 1cm long line drawn on it on the projector to project an image on the wall chart  Focus the projector so that a sharp shadow of the line appears on the screen  Measure the length of the image accurately with a metal ruler or measuring tape  Adjust the position of the projector till a 7X magnification of the 1cm long line is obtained. Film Properties 25 HPL/CSE/TECH/SE/4.4.4/01/03/OHPV confidential Test Specimens A total film test area of 1520 sq.cm (240 sq.in) is employed for the testing, the area being divided into six specimens of 40 sq. in (8” X 5”) each. The HDPE film samples shall be prepared by blown film extrusion and shall be of thickness 10 microns. For R5801, however, the film samples of thickness 40 microns shall be prepared. Procedure  Mark out an area of 8”X5” on each film specimen using a marker.  Place the film on the projector and view its image on the screen.  Circle the gels on the film using a fine tip marker.  Ascertain the size of the gels by placing the standard sizing template on each surface defect image projected on the screen. The size of the gel is taken as that closely matching a given reference line on the template.  Record the number of gels, classified according to their size for each test specimen.  Depending on specifications requirements, defects sizes may be classified as <= 0.2mm & >0.2mm  Weigh the test specimens. 7. Calculation Total Weight of all the test samples in gm.=W N1 = Total number of small (<= 0.2mm) gels N2 = Total number of large (>0.2mm) gels Number of small gels per unit film weight = A = N1 / W (in numbers / gm) Number of large gels per unit film weight = A = N2 / W (in numbers / gm) A = A + B/10 The gel rating of the film shall be as per the tables below: a a ≤ 1.5 1.5 < a ≤ 3.0 3.0 < a ≤ 10 10 < a ≤ 20 20 < a ≤ 30 30 < a ≤ 40 40 < a Gel Rating 7+ 7 5+ 5 53 1 8. Reporting  Complete identification of the sample  Date of test  The respective numbers of large & small fish eyes in number / gm  Gel rating 9. References Film Properties 26 HPL/CSE/TECH/SE/4.4.4/01/03/OHPV  ASTM D 3351  HZ – A – 320 – 1 Film Properties confidential 27