ISO 11171 Calibration Seminar ISO 11171校定讲座

Course Instructor Craig Gustafson

Particles & Particle Counter颗粒与颗粒计数

• Particle contamination is recognized as the most destructive to oil and machine

颗粒污染被认为是对油品和机器最具危害的因素

– “microscopic wreaking crews 微小的复仇者”– 75% of failures are due to contamination

75%的故障是由污染引起

• Leading indicator of machine condition 机器状况的主要指标

• The “Invisible Filter 无形的过滤器”• The “Contamination Thermometer 污染指示计”

Number of particles in 1ppm (mg/l)

1ppm浓度流体中的颗粒数量

ISO 11171 - SRM 2806 (2.8mg/l)

108,400 particles/ml @ 1µm1mg/l or 1ppm = 38,714 particles/ml

513.7 particles/ml @ 10µm1mg/l or 1ppm = 183.5 particle/ml

1 µm

10 µm

Very sensitive technique非常灵敏的技术

• excellent early warning 完善的早期预警

• (sample handling试样处理)Accepted - National & International Standards被多个国家及国际标准认可

Simple, robust, fast and precise简单，有效，快速，精确

(Does not give accurate size data - mV response不给出准确的颗粒径数据-毫伏响应)(Responds to light interaction响应感光作用)• Hard and soft particle 硬的和软的颗粒

(emulsions, bubbles 乳胶球，气泡)(Field Sampling现场取样 - obtaining a representative sample获取具有代表性的试样)

Principle of Operation工作原理

Sensor Technologies传感器技术(simplified简介)

• Light blocking光遮挡

• Near forward scatter近距向前散射

Hiac 8011 System 系统

Test date: 11 April 2000 Operator: D. Hoagland

ISO 11171 Calibration校定

Testing测试

Results结果

Summary of ISO 11171 Test ResultsISO 11171 测试结果简要分析

Coefficient of Variation 变量系数 (COV) 0.28%Coincidence Limit 重叠限制 (counts/ml) 10174Flow Rate Limits流率限制

Lower 下限 (ml/minute) 45 Upper 上限 (ml/minute) 77Resolution 分辨率 (per cent%) 6.8%Counting Accuracy 计数准确度 PassFinal Calibration Data 最终校正数据 See Graph见曲线图

Sample Volume Accuracy取样体积准确度

Run测试

Buret滴定

(0)Buret滴定

(100)

SampleVolume取样体积

(ml)

1 20.1 10.0 10.1

2 39.1 29.1 10.0

3 44.1 34.2 9.9

Average 10.0

Coefficient of Variation变化系数 (COV)

Run测试 Channel 1 Counts通道1计数值

1 863522 857433 861194 861395 85872

Std Deviation标准偏差 239.6320095

Coincidence Limit重叠限制

(counts/mL)Conc. Run 1 Run 2 Run 3 Run 4 Run 5 Average Error (Dq)10% 3047 3034 3055 3051 3057 3048.8 0.8%20% 5483 5457 5482 5408 5446 5455.2 1.4%30% 7545 7516 7452 7427 7434 7474.8 1.6%40% 9303 9226 9242 9224 9209 9240.8 1.0%50% 10698 10598 10618 10596 10551 10612.2 1.4%60% 11922 11918 11891 11936 11944 11922.2 0.4%70% 13003 12874 12910 12855 12860 12900.4 1.1%80% 13981 13920 13922 13944 13862 13925.8 0.9%90% 15046 14894 14915 14908 14919 14936.4 1.0%100% 15657 15643 15597 15523 15556 15595.2 0.9%110% 16383 16383 16393 16419 16437 16403.0 0.3%120% 17361 17243 17197 17135 17121 17211.4 1.4%130% 17743 17593 17603 17612 17545 17619.2 1.1%140% 18127 18057 18086 18061 18084 18083.0 0.4%150% 18563 18539 18547 18656 18775 18616.0 1.3%

Coincidence Limits重叠限制

slope2060

average10-40%

2645

correlationcoefficient0.9726522

intercept2918

Conc Limit10174

Conc Actual实际值 Calculated计算值 Minus减 5% Deviation偏差

0 0.0 0 0 X10 3049 3049 2897 X20 5455 5455 5182 X30 7475 7475 7101 X40 9241 9241 8779 X50 10612 11454 10881 -7.3%60 11922 13514 12838 -11.8%

1 2 3 4 5 6 7

ActualIdealMinus 5%

Flow Rate Limit Data流率限制数据

Flow RateError

36 48 60 72 848.7% 3.3% 0.0% -3.6% -6.6%

Flow Rate Run 1 Run 2 Run 3 Run 4 Run5 Average Variation Error36 93646 92992 93004 93236 94942 93564 2.1% 8.7%48 88740 88526 89202 89655 88447 88914 1.4% 3.3%60 86352 85743 86119 86139 85872 86045 0.7% 0.0%72 82667 83056 82855 82984 83030 82918 0.5% -3.6%84 80888 79928 80086 80467 80487 80371 1.2% -6.6%

Flow Rate Limits流率限制-100%

-75%

-50%

-25%

0%

25%

50%

75%

100%

20 30 40 50 60 70 80

Flow Rate流率 (ml/minute)

Erro

r误差

-15%

-10%

-5%

0%

5%

10%

15%

20 30 40 50 60 70 80

Flow Rate流率 (ml/minute)

Erro

r误差

Lower Limit下限

45

Upper Limit上限

77

Resolution Determination 分辨率的确定

RMCA Methodology方法Moving Window Methodology方法

准备乳胶球试样

准备颗粒计数器

分析试样

第2,3通道差别大于3%？

通道间的差别最小？

重新调整前4个通道

维修或更换颗粒计数器

是

否

是

否

为前5个通道

确定新设置

分析乳胶球试样

计算分辨率

否

是

分辨率<10%? 分辨率确定完成

准备乳胶球试样

准备颗粒计数器

分析试样

是

否

分辨率<10%?

分辨率确定完成

Sensor Resolution传感器的分辨率(sensor signal output传感器信号输出)

Poor resolution较差的分辨率

Good resolution较好的分辨率

Perfect resolution最好的分辨率

Excessive

Δ VZero Δ VAcceptable

Δ V

Beam Profile Impact On Resolution

激光束质量对分辨率的影响

•Inconsistent laser intensity in the beam profile can cause sizing errors.光束剖面中不均匀的光强

度会引起尺度误差

• Illuminating the view volume with a beam of uniform intensity will produce better resolution.测量区域中光强度

均匀的激光束将产生更好的分辨率

Poor Beam Profile较差的光束剖面光强分布

Peak Intensity峰值强度

Peak Intensity峰值强度

Particles scatter or block varying amounts of light, resulting in sizing errors.在光束中的颗粒散射或遮挡不同等量的光，导致测量尺度的误差

Particles scatter or block varying amounts of light, resulting in sizing errors.在光束中的颗粒散射或遮挡不同等量的光，导致测量尺度的误差

Bea

m P

ower光强

Beam cross section光束截面

Less than peak intensity小于峰值强度

Less than peak intensity小于峰值强度

Uniform Beam Profile均匀的光束剖面光强分布

Bea

m P

ower

光强

Beam cross section光束截面

Uniform Intensity均匀的光强分布

Peak Intensity峰值强度

Peak Intensity峰值强度

Variations in light intensity are minimal, resulting in

accurate sizing(high resolution).

光强的变化最小，测量尺度准确（分辨率高）

Variations in light intensity are minimal, resulting in

accurate sizing(high resolution).

光强的变化最小，测量尺度准确（分辨率高）

When is resolution test required何时需要做分辨率测试

• New or existing system requiring ISO 11171 需要做ISO 11171标准的新系统或已有系统

• Sensor optics repaired or adjusted 传感器光学部件经过维修或调整

• Sensor or counter electronics repaired or adjusted

传感器或计数器的电子线路经过维修或调整

Resolution Determination分辨率的确定

准备乳胶球试样

准备颗粒计数器

分析试样

第2,3通道的差别>3%？

是

否

是

否

通道之间的差别最小？

重新调整前4个通道

否维修或更换颗粒计数器 是

分辨率<10%?

确定前5个通

道的新设置

分析乳胶球试样

计算分辨率

分辨率确定完成

Preparing sample准备试样

• Prepare AOT in concentrate, and dilution

• Concentration of spheres in AOT-5606AOT-5606中的圆球浓度

• Blend spheres into final concentration 混合圆球至最终浓度

Modified Half-Count Method已修改的“半数”方法

• Prepare particle counter ~ 准备颗粒计数器

– Differential count mode 设置为差分计数方式

– Channel A @ 1.5x noise level 通道A：1.5x噪声值

– Channel C @ 10m(c) + 20% 通道C：10m(c) + 20%– Channel B @ 0.72x channel C 通道B：0.72x通道C– Channel D @ 1.32x channel C 通道D：1.32x通道C

Calculate results计算结果

• Calculate results, adjust channels until D ≤ 3% or at minimum value

计算结果，调整通道直到D值≤ 3% 或为最小值

Resolution Tests分辨率测试

Channel Threshold (mv) Cum Counts Diff Counts D Threshold (mv) Cum Counts Diff Counts D1 12.0 X X 12.0 X X2 169.2 52275 16349 48.0% 180.0 54680 32916 -91.8%3 235.0 35926 31438 250.0 21764 171594 310.2 4488 X 330.0 4605 X

Channel Threshold (mv) Cum Counts Diff Counts D Threshold (mv) Cum Counts Diff Counts D1 12.0 X X 12.0 X X2 172.8 36941 15773 16.7% 174.2 37679 17749 0.0%3 240.0 21168 18945 242.0 19930 177554 316.8 2223 X 319.4 2175 X

Channel Threshold (mv) Cum Counts Diff Counts D Threshold (mv) Cum Counts Diff Counts D1 12.0 X X 12.0 X X2 174.6 36170 16269 7.0% 175.0 42517 21577 -24.6%3 242.5 19901 17495 243.0 20940 173224 320.1 2406 X 320.8 3618 X

Channel Threshold (mv) Cum Counts Diff Counts D Threshold (mv) Cum Counts Diff Counts D1 12.0 X X 12.0 X X2 173.9 57679 26800 -3.7% 173.2 60652 27171 5.7%3 241.5 30879 25856 240.5 33481 288014 318.8 5023 X 317.5 4680 X

TEST 1 TEST 2

TEST 3 TEST 4

TEST 5 TEST 6

TEST 7 TEST 8

8011-3941 Sales no: 26881 RESOLUTION 6.8%Fluid: 10um Spheres in 5606 oilNoise (mv): 8.0

Resolution Check分辨率检查

Channel Threshold (mv) Run 1 Run 2 Run 3 Run 4 Run 51 12.0 64137 64303 64801 64651 649032 173.5 58185 58362 58818 58572 587833 241.0 32230 32297 32181 31910 320924 318.1 4491 4524 4422 4472 4628

Average Variation Max variation Diff Counts D64559 1.2% 11.3% X 4.5%58544 1.1% 11.3% 2640232142 1.2% 11.3% 27634.64507 4.6% 11.3% X

Resolution Determination分辨率的确定

Prepare particle counter ~ 准备颗粒计数器

– Differential count mode 差分计数方式

– Channel A @ 0.72x channel C 通道A设为 0.72x通道C

– Channel B @ 0.9x determined size 通道B设为 0.9x确定粒径

– Channel C @ determined size 通道C设为 确定粒径

– Channel D @ 1.1x determined size 通道D设为1.1x 确定粒径

– Channel E @ 1.32x channel C 通道E设为1.32x通道C

Resolution Determination分辨率的确定

• Left and right side variation ~ 左右两侧的变化

Resolution Determination分辨率的确定

• Corrected for deviation of spheres ~ 球体偏差修正

Resolution分辨率

Channel Threshold (mv) um© Run 1 Run 2 Run 3 Run 4 Run 51 12 4432.4 4443.4 4435.8 4401 4408.92 173.5 3993.5 4004.9 4031.7 3988.3 40073 211.2 10.22 3631 3635.1 3656.8 3623.8 3638.94 241.0 11.35 2198 2193.1 2223.5 2195 2208.35 265.7 12.49 629.1 630.7 633.4 626.1 6266 318.1 341.2 341.3 343.9 338.9 340.7

Average Variation Max variation Diff Counts4424.3 1.0% 419.24005.1 1.1% 11.3% 368.13637.0 0.9% 11.3% 1433.52203.5 1.4% 11.3% 1574.42629.1 1.2% 11.3% 287.9341.2 1.5% 11.3% X

SL SR d0.87029939 0.76283257 11.35

RL RR RESOLUTION6.8% 5.7% 6.8%

Shperes SD 0.4

Resolution Determination 分辨率的确定

RMCA Methodology方法Moving Window Methodology方法

准备乳胶球试样

准备颗粒计数器

分析试样

第2,3通道差别大于3%？

通道间的差别最小？

重新调整前4个通道

维修或更换颗粒计数器

是

否

是

否

为前5个通道

确定新设置

分析乳胶球试样

计算分辨率

否

是

分辨率<10%? 分辨率确定完成

准备乳胶球试样

准备颗粒计数器

分析试样

是

否

分辨率<10%?

分辨率确定完成

Accuracy Verification准确度验证

Run 1 Run 2 Run 3 Run 4 Run 56845 6878.6 6885.5 6877.3 6854.4

4099.6 4061.6 4045.5 4045.9 4008.62097.8 2066.5 2038.7 2042.3 2016.1

501 483.6 472.2 464 463.5123 111.1 105 104 105.312.5 8.4 7.8 7.4 6.9

SAMPLE 1

Run 1 Run 2 Run 3 Run 4 Run 56901.5 6892.7 6878.8 6845 6845.24100.5 4042.9 4075.5 4019.9 4025.12067.4 2030.6 2068.2 2037.2 2018474.3 465 478.2 466.3 474.4111.1 109.5 106.7 104.9 110.28.4 8.7 7.3 8.8 9.4

SAMPLE 2

Run 1 Run 2 Run 3 Run 4 Run 56877.1 6848.9 6829.2 6806.5 6841.74014.5 4007.1 4000.7 3982.6 39902042.3 2008.5 2026.4 2004.2 2018.1483.7 463.5 463 452.7 465.8112.3 105.2 104.7 105.8 106.58.4 7.9 8.6 7.8 7.3

SAMPLE 38011-3941Fluid: UFTD-oil (1mg/l) P/F Pass

ChannelSize um

(c) Average AVG MINAVG MAX Std Dev COV

COV MAX

1 4 6860.5 5400 8100 26.32032 0.38% 4.0%2 5 4034.7 3300 4500 37.10017 0.92% 4.1%3 6 2038.8 1500 2500 26.28191 1.29% 4.3%4 8 471.4 280 760 11.76781 2.50% 5.7%5 10 108.4 58 220 4.908719 4.53% X6 14 8.4 4.1 19 1.329053 15.87% X

26881

Counts/mL

Sales No:

1

10

100

1000

10000

100000

10 100 1000 10000

millivolts

coun

ts/m

l

Size Calibration粒径校正

COUNT DATAMV COUNTS12.0 821515.0 699218.7 602123.4 521729.2 456136.5 395345.6 331056.9 285271.1 235588.8 1868111.0 1480138.6 1070173.1 729216.3 456270.2 236337.5 118421.5 60.1526.5 26.7657.7 13.0

DATAUM(c)3.503.804.004.304.604.905.305.606.056.607.157.959.0010.4012.7015.7019.1523.4027.40

1

10

100

1000

1 10 100

um (c)

mill

ivol

ts

Final Calibration最终校定

Channel mv Size uM (c) Run 1 Run 2 Run 3 Run 4 Run 5 Average Variation Error1 18.7 4 5919.4 5881.4 5872.1 5875.3 5894.1 5888.5 0.8% -3.4%2 69.7 6 2327 2313.7 2301 2298.6 2290.8 2306.2 1.6% -3.7%3 299.8 14 177.6 177.3 172.8 165.6 164.8 171.6 7.5% 0.7%4 585.6 25 20 20.8 17.6 18.1 17.5 18.8 17.6% -5.8%5 1340 50 1.1 0.6 1.3 0.7 0.4 0.8 X X6 2716 100 0 0 0 0 0 X X X

ISO MTDMV COUNTS UM�18.7 5888.5 469.7 2306.2 6299.8 171.6 14585.6 18.8 251340.2 0.8 502715.7 X 100

8011-3941Sales no. 8

Fluid3-11-C

Threshold noise (mv)26881ISO MTD 2.8 mg/lNIST 2806 3-78-C

1

10

100

1000

10000

1 10 100

Size uM (c)

Mill

ivol

ts

Summary of ISO 11171 Test ResultsISO 11171 测试结果简要分析Threshold Noise 阈值噪声 (mv) 8.0Actual Sample Volume 实际试样体积(ml) 10.00Coefficient of Variation 变化系数 (COV) 0.28%Coincidence Limit 重叠限制 (counts/ml) 10174Flow Rate Limits 流率限制

Lower 下限(ml/minute) 45 Upper 上限(ml/minute) 77Resolution 分辨率(per cent%) 6.8%Counting Accuracy 计数准确度 Pass 合格

Final Calibration Data 最终校定数据 See Graph见图

Types of Calibration 校定的类型Hydraulic Applications 液压应用

• ACFTD (based upon ISO 4402)

• MTD (based upon ISO 11171)

• ISO 11171 (Full conformance)

• ISO 11171 (Secondary Calibration)

Types of Calibration Fluids校定流体的类型

• NIST Traceable kit #2084498-0NIST 可追溯的校定流体

• MTD #650-650-0010

• Count Accuracy #2084499-01计数精确

• ACFTD kit #640-0041 AC粉尘校正液

ISO 11171 Calibration Seminar校正会议

Course Instructor Craig Gustafson

References参考

• ISO 11171: 1999 – Hydraulic fluid power – Calibration of particle counter for liquids • ISO 11943:1999 – Hydraulic fluid power – On-line..Calibration and Validation• ISO 4402 – Hydraulic fluid power – Calibration particle counters using ACFTD• ISO 4406 – Hydraulic fluid power – Method for coding level of contamination • NAS 1638 – Cleanliness requirements, Hydraulic Systems• ISO 11171 Seminar and Workshop NFPA, FTI, PSI – April 2000• Enumerator - Pacific Scientific Instruments P Rossi• Fluid Power Update - Pacific Scientific Instruments C Gustafson• Distribution & Efficiency - Pacific Scientific Instruments J Contreras