IEC 60811-4-1 Testing methods for Insulating and sheathing materials of electric and optical cables

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IEC 60811-4-1 Insulating and sheathing materials of electric and optical cables – Common test methods:

Methods specific to polyethylene and polypropylene compounds – Resistance to environmental stress cracking – Measurement of the melt flow index – Carbon black and/or mineral filler content measurement in polyethylene by direct combustion - Measurement of carbon black content by thermogravimetric analysis (TGA) – Assessment of carbon black dispersion in polyethylene using a microscope

IEC 60811-4-1:2004 specifying five specialized test methods for polyethylene (PE) and polypropylene (PP) compounds used as insulating and sheathing materials in electric and optical fiber cables for power distribution, telecommunications, shipboard, and offshore applications.

Core Mechanical Test Methods and Testing equipment recommend of IEC 60811-4-1:

Test Method	Description
Resistance to Environmental Stress Cracking (ESCR)	Evaluates material's resistance to cracking under combined chemical and mechanical stress
Melt Flow Index (MFI) Measurement	Determines polymer's flow properties under specified temperature and load conditions
Carbon Black/Mineral Filler Content (Direct Combustion)	Quantifies filler content in polyethylene via controlled combustion
Carbon Black Content (Thermogravimetric Analysis, TGA)	Measures carbon black content using thermal decomposition analysis
Carbon Black Dispersion Assessment (Microscope Method)	Evaluates uniformity of carbon black distribution in polyethylene matrix

Details IEC 60811-4-1 test methods, specimen, test procedures, testing equipments introduction:

Environmental Stress Cracking (ESCR) Test

(refer ISO 4599, ASTM D1693)

Test Equipment: Environmental Stress Cracking Apparatus

Stress-cracking reagent (5% Igepal CO-630 in distilled water)

Test tubes with stoppers

Specimen holders/clamps for applying controlled stress

Notch cutter (for notched specimens).

Thermostatically controlled water bath (50°C ± 1°C)

Magnifying glass or microscope (10× magnification).

IEC 60811-4-1 Testing methods for Insulating and sheathing materials of electric and optical cables

Test Specimen:

Materials: Must be the original granules of the cable sheath.

Preparation: About 90g of granules are molded at 165-170°C under a pressure of 50-200 kN for 2 minutes to form test pieces of approximately 150mm x 180mm x (3.3±0.1)mm.

Conditioning: The test pieces need to be heat-treated at specific temperatures (depending on density: low density 145°C, medium density 155°C, high density 165°C) for 1 hour, and then cooled programmatically to (29±1)°C at a rate of (5±2) K/h.

Final ESCR test samples: Cut 10 rectangular strips of (38.0±2.5)mm x (13.0±0.8)mm from the treated test pieces. Their thickness (C) and notch depth (D) have strict requirements according to the material density.

Main ESCR Test steps:

Use a dedicated notching device to make a notch of specified depth at the center along the length of each specimen.

Use a bending clamping device to bend 10 specimens simultaneously within 30-35 seconds.

Use a transfer tool to place the bent specimens into a slotted brass specimen holder, then put them together into a glass test tube.

Pour the reagent of specified concentration into the test tube (100% concentration for step A, 10% aqueous solution for step B).

Place the test tube into a thermostatic container at (50±0.5)°C and start timing.

Check regularly and record the time when the first crack appears (considered as the failure of the specimen).

Carbon Black Content Carbon (Direct Combustion Method)

(refer ISO 6408)

Test equipment: Carbon black content tester:

Tube furnace, rigid glass/quartz/ceramic combustion tube (length ~400mm).

Stopper with thermometer and inlet.

Combustion boat.

High-purity nitrogen, oxygen/air gas source and flow control.

Analytical balance (accuracy 0.0001g).

Test Specimen:

Sample requirements: Remove the insulation or sheath material from the cable and cut it into small pieces with any dimension not exceeding 5mm. Take about 1.0g of the sample.

Main experimental steps:

Place the sample into a pre-weighed crucible and accurately weigh it (mass A).

Place the crucible into the combustion tube and pass nitrogen gas through it (flow rate 1.7 L/min).

Put the combustion tube into the furnace and heat according to the program: 10 minutes to 300-350°C, then another 10 minutes to ~450°C, then 10 minutes to (600±5)°C, and hold for 10 minutes.

This process decomposes the polymer.

After cooling, weigh the total mass of the crucible and residue (mass B, i.e., the total filler content).

Place the crucible back into the tube, and at (600±20)°C, pass air or oxygen through it to burn off the carbon black.

After cooling, weigh again (mass C, i.e., the mineral filler content).

Melt Flow Index (MFI) Test

(refer ISO 1133, ASTM D1238)

Test equipment: Melt flow indexer with:

Heating barrel (temperature control: ±0.5°C)

Standard die (2.095mm diameter × 8.000mm length)

Piston with specified weights (2.16kg, 5.0kg, etc.)

Stopwatch (±0.1s accuracy)

Balance (±0.001g precision)

Sample requirements: Insulation or sheath material removed from the cable, cut into small pieces with any dimension not exceeding 3mm.

Main Experimental Steps (Method A):

Clean and preheat the extruder (barrel and piston) to (190±0.5)°C.

Add one sample (about 4-5 g).

After feeding for 4 minutes, apply a load of 21.2 N on the piston to extrude the material from the die.

Use a sharp tool to cut the extruded material at specified time intervals (ranging from 60 s to 240 s according to the estimated melt index, see Table 1).

Weigh each cut segment and calculate the average value.

Carbon Black Dispersion Assessment (Microscope Method)

(refer ISO 18553)

Test equipment: Carbon Black Dispersion Tester

Optical microscope (400× magnification) with brightfield illumination

Microtome for preparing thin sections (5-10μm thickness)

Mounting medium and slides

Dispersion rating scale (5-point scale: 1=excellent, 5=poor)

Sample requirements:

Suitable for polyethylene mixtures or extrusion layers (such as sheaths) with a carbon black content of less than 3%. There are two methods for sample preparation:

Compression method: Mainly used for pellet mixtures, thin sheets are prepared by hot pressing.

Slicing method: Thin slices are cut from the extrusion layer using a microtome.

Main test Steps:

Prepare thin sections (5-10μm) using a microtome;

Mount sections on microscope slides;

Examine at least 5 different fields of view per specimen;

Rate dispersion quality based on:

Size and distribution of carbon black aggregates;

Presence of undispersed carbon black agglomerates;

Degree of matrix wetting;

Assign a numerical rating (1-5) according to standard criteria.

Related Standards:

IEC 60811-4-1:2004 is part of the IEC 60811 series and references several other standards:

Related Standard	Description
IEC 60811-1-1	General test methods for cable materials
IEC 60811-511	Melt flow index measurement (replaces IEC 60811-4-1 section 10). Electric and optical fibre cables - Test methods for non-metallic materials - Part 511: Mechanical tests - Measurement of the melt flow index of polyethylene and polypropylene compounds.
IEC 60811-605	Carbon black/mineral filler content measurement (replaces direct combustion method)
IEC 60811-607	Carbon black dispersion assessment (replaces microscope method)
ISO 4599	Environmental stress cracking resistance of plastics
ISO 1133	Melt flow rate of thermoplastics
ISO 18553	Carbon black dispersion in plastics

ESC-95 Environmental Stress Cracking Resistance (ESCR) Apparatus determines the susceptibility of ethylene plastics to stress-cracking when exposed to different environments such as soaps, wetting agents, oils and detergents.

Carbon black content tester is used to measure the carbon content in PE, PP, PB etc. , sample under nitrogen condition, through high temperature pyrolysis, then measure the weight to get the carbon level.

Melt flow index tester is for melt mass-flow rate (MFR) and the melt volume-flow rate (MVR),to measure the melt mass flow rate of thermoplastic plastics under specific temperatures and pressures, reflecting the flow performance of materials through standardized testing.

Carbon black dispersion tester is designed according ISO 18533 standard, used to measure the carbon black dispersion in polyolefin pipes, fittings and compounds. Adaptive to measuring software, and the microscope, measure the size, form, dispersion condition of the carbon black granule.

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