Performing Particle Counting on Opaque and Heavily Contaminated Samples
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1 Performing Particle Counting on Opaque and Heavily Contaminated Samples Author Bill Quesnel / CINRG Systems Inc., Burlington, ON, CANADA Co-Author Alistair Geach / WearCheck Canada Inc., Burlington, ON, CANADA CSO-1
2 What is the biggest issue with Particle Count Testing? Reproducibility of Results is Questionable! CSO-2
3 Why? Different Methods Employed by Commercial Laboratories each with their sources of variability; ASTM F312 Particle Debris Patch & Visual Count (Microscopic) o Time consuming and expensive o Operator dependent o Precision of measurement is questionable No Method Pore Blockage o Current technology is now obsolete o Fairly accurate for total particles, but high error for particle size distribution ISO 4406:1987 Optical Particle Count 5µm/15µm.maybe 2µm/5µm/15µm o Discontinued method o Many instruments in the field may still be calibrated to this method o Coincidence - cannot count dark or opaque samples, or fluids with water > 0.03% o Soft particle effects from oxidative byproducts (varnish precursors, some additives) ISO 4406:1999 Optical Particle Count 4µm/6µm/14µm o Coincidence - cannot count dark or opaque samples, or fluids with water > 0.03% o Soft particle effects from oxidative byproducts (varnish precursors, some additives) CSO-3
4 Particle Debris Patch Particle Counting Opaque & Heavily Contaminated Samples Too much water Too dark Too dirty Particle Debris Patch Microscopic Examination Cleanliness Guesstimation ISO 21/19/16? CSO-4
5 What Did we Study? Diluted Samples (Automatic) vs. Undiluted Samples (Manual) Samples with a lot of water contamination Soft Particle Effects - Samples with oxidative byproducts (varnish) Coincidence Issues - Samples with a whole lot of particulate Automatic Diluted Samples Testing Repeatability CSO-6
6 Hiac 8012 vs. CINRG CS-APC-2 Undiluted Diluted 1:1 CSO-7
7 Processing Samples Water Contamination - Laboratory Samples CSO-8
8 Processing Samples Water Contamination Sample ID % Water 4µm (c) 6µm (c) 14µm (c) 21µm (c) 38µm (c) 70µm (c) Cleanliness Code RM T 0.1% /25/24 Table 2 Testing results from trial of 0.1% water in MIL-H-5606 oil using 100% Toluene as a solvent. CSO-9
9 Processing Samples Water Contamination Figure 5 0.1% water contamination using 100% toluene as a diluent vs. 0.5% water contamination using 75% toluene / 25% isopropanol as a diluent. CSO-10
10 Processing Samples Water Contamination Sample ID % Water 4µm (c) 6µm (c) 14µm (c) 21µm (c) 38µm (c) 70µm (c) Cleanliness Code RM % /18/11 RM % /18/11 RM % /18/11 RM % /18/11 RM8632_20 2.0% /18/11 RM8632_25 2.5% /22/19 RM8632_30 3.0% /24/23 Table 1 Testing results from trial of water in MIL-H-5606 oil using 75% Toluene/25% Iso-propanol as a solvent. CSO-11
11 2.0% water Particle Counting Opaque & Heavily Contaminated Samples Processing Samples Water Contamination Figure 4 Individual micron channel results from trial of 0.5% to 3.0% water in MIL-H oil using 75% Toluene / 25% Iso-propanol as a solvent. CSO-12
12 Processing Samples Water Contamination in Used Oil Samples CSO-13
13 Processing Samples - Water Contamination in Used Oil Samples Samples As Received Samples After Shaking % 1.6% 1.35% 0.35% Samples Before Dilution & Samples After Dilution CSO-14
14 Processing Samples Water Contamination Table 3a Testing results from used oil samples with high concentrations of free and emulsified water on the Hiac 8012 undiluted. Sample ID Free Water % Water Dilution Oil:Solvent 4µm (c) 6µm (c) 14µm (c) 21µm (c) 38µm (c) 70µm (c) Cleanliness Code % 14.76% none /0.7/ % 1.60% none /0.7/ <1% 1.35% none /0.7/ <1% 0.35% none /0.7/0.7 Table 3b Used oil samples with high concentrations of free and emulsified water on the CINRG CS-APC-2 using 75% Toluene / 25% Isopropanol as a solvent. Sample ID Free Water % Water Dilution Oil:Solvent 4µm (c) 6µm (c) 14µm (c) 21µm (c) 38µm (c) 70µm (c) Cleanliness Code % 14.76% 1: /19/ % 1.60% 1: /18/ <1% 1.35% 1: /19/ <1% 0.35% 1: /19/16 CSO-15
15 2.0% water Particle Counting Opaque & Heavily Contaminated Samples Processing Samples Water Contamination Figure 4 Individual micron channel results from trial of 0.5% to 3.0% water in MIL-H oil using 75% Toluene / 25% Isopropanol as a solvent. CSO-16
16 Processing Samples Opaque Samples CSO-17
17 Processing Samples Opaque Samples (Castrol Optigear A 320) Count Data 4µm (c) 6µm (c) 14µm (c) 21µm (c) 38µm (c) 70µm (c) Cleanliness Code Undiluted Sample /23/13 Diluted Sample(1:1) /17/13 Table 4 Particle Testing results for both diluted and undiluted preparation for sample Count Data 4µm (c) 6µm (c) 14µm (c) 21µm (c) 38µm (c) 70µm (c) Cleanliness Code Undiluted Sample /22/14 Diluted Sample(1:1) /15/12 Table 5 Particle Testing results for both diluted and undiluted preparation for sample CSO-18
18 Processing Samples Opaque Samples (Castrol Optigear A 320) undiluted diluted 1:1 Figure 8 Comparison of undiluted particle counts on the Hiac Royco SDS particle counter versus diluted particle counts for Castrol Optigear Synthetic A ISO 320 on the CS-APC-2 particle counter. CSO-19
19 Sample Sample Color Image with Visibility Scale Color Image with Visibility Scale 23/23/13 or 19/17/13? 23/22/14 or 19/15/12? Particle Debris 100X magnification Particle Debris 100X magnification CSO-20
20 Table 6: Particle count data from the Hiac 8012 particle counter on wind turbine gearbox used oil samples using Castrol Optigear Synthetic A 320 gear oil (undiluted). NOTE: Coinc. Ftr is the calculated coincidence factor given the 4 micron count. Sample ID Coinc. Ftr MPC 4µm (c) 6µm (c) 14µm (c) 21µm (c) 38µm (c) 70µm (c) ISO Code /17/ /17/ /19/ /18/ /15/ /23/ /22/ /16/ /23/ /16/ /16/ /15/ /17/ /14/ /18/ /15/ /19/ /22/ /15/ /20/ /19/ /15/12 CSO-21
21 Table 7: Particle count data from the CINRG CS-APC-2 particle counter on wind turbine gearbox used oil samples using Castrol Optigear Synthetic A 320 gear oil (samples diluted 1:1 with 75% Toluene / 25% Isopropanol as a solvent). NOTE: Coinc. Ftr is the calculated coincidence factor given the 4 micron count count. Sample ID Coinc. Ftr. MPC 4µm (c) 6µm (c) 14µm (c) 21µm (c) 38µm (c) 70µm (c) ISO Code /16/ /14/ /19/ /15/ /14/ /17/ /16/ /14/ /15/ /15/ /15/ /15/ /15/ /14/ /16/ /15/ /17/ /16/ /14/ /20/ /19/ /15/11 CSO-22
22 MPC Images / Results (MPC = 8) (MPC = 157) (MPC = 29) (MPC = 73) (MPC = 29) (MPC = 53) Figure 10: MPC patches for a variety of the gearbox samples tested CSO-23
23 HIAC 8012 CINRG CS-APC-2 undiluted diluted 1:1 CSO-24
24 HIAC 8012 undiluted CINRG CS-APC-2 diluted 1:1 CSO-25
25 Particle Debris Patches (MPC = 159) PDF / Kerosene (ISO 23/23/21) PDF / Toluene (ISO 17/15/11) (MPC = 47) PDF / Kerosene (ISO 23/22/17) PDF / Toluene (ISO 20/16/12) Figure 11: Particle Debris patches for two of the gearbox samples tested comparing solvents. CSO-26
26 Processing Samples Opaque Samples Processing Samples Heavily Contamination Samples CSO-27
27 Processing Samples Heavily Contaminated (Gross Particulate Concentration) Count Data 4µm (c) 6µm (c) 14µm (c) 21µm (c) 38µm (c) 70µm (c) Cleanliness Code Current /27/22 Historical /27/23 Historical /27/23 Table 10 Particle Testing results for heavily contaminated gearbox samples at 1:30 dilution ratio. CSO-28
28 Figure 17 A ferrogram (top) of the most current gearbox sample illustrating the high quantity of metal present in the oil (200x magnification, bichromatic light, sample prepared with 1:10 dilution). A particle debris patch (bottom left) and sample visual clarity image (bottom right) of the most current gearbox sample illustrating the high quantity of metal present in the oil (particle debris patch 100x magnification, reflected white light) CSO-29
29 Processing Samples Heavily Contaminated (Gross Particulate Concentration) Figure 15 Trend of 3 samples over a 5 month period from a heavily contaminated gearbox. CSO-30
30 Processing Samples Repeatability CSO-31
31 Repeatability Particle Counting Opaque & Heavily Contaminated Samples HIAC 8012 CINRG CS-APC-2 Internal Standard 2010 n:149 Internal Standard 2014 n:247 CSO-32
32 Repeatability CINRG-CS-APC2 Process Control Standard (over a 2-month period) 4µm (c) 6µm (c) CSO-33
33 Future Study Reproducibility of Particle Count Results using the CINRG CS-APC-2 Instrument 6 Instruments in 4 countries Thank-you! CSO-34
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