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17th World Conference on Nondestructive Testing, 25-28 Oct 2008, Shanghai, China The Fluorescence Penetrant Agent Manufacture and Its Wastewater Treatment Zhenwang LIN 1 Zhenlu CHEN 1 Dongsheng LI 2 Jiangpai LI 3 Zhonglin CHEN 1 1 Xiamen Jimei Xincheng NDT Manage Department Rm.103,No.13,Fangzhi Road,Xinglin,Jimei District,Xiamen 361022, China Tel:86-592-5287678.Fax:86-592-6259989 E-Mail : [email protected]; E-Mail :[email protected] 2 Honeywell TAECO Aerospace (Xiamen) Co.,Ltd , Xiamen, China E-Mail :[email protected] 3 Xiamen Airline Company Limited, Xiamen, China Abstract The author had spent decades in theoretical research and experiments in manufacturing water washable types and post emulsifiable fluorescence penetration agentemulsifiersdevelopers of various types etc. Thus the performance of this product complied with the specification and requirements of People Republic of China aerospace industry standard HB7681-2000 and US aerospace material specification AMS 2644E standard. The Index performance of some product peers excelled and achieved international standards compared with similar product types. The author researched and explored the product in wastewater treatment with fluorescence penetration test process. By separation of oil from water and emulsion breakage and then finally achieving transparency and clear of the water. The wastewater of C O D Cr value ranged from 10000 to 20000. After primary treatment, the clear water of C O D Cr value reduced between 50 to 300. Whereby achieving an environmental protection level 3 effluent standards. The waste oil can be further reused optimized by further treatment. Key word: fluorescence penetrant agent; performance; wastewater treatment; resource recovery 1. Introduction The author had written several thesis related to penetrate topics 1 )( 2 )( 3 and conducted laboratory experiments and theoretical researches for decades and had researched and manufactured water washable types and post emulsifiable types fluorescence penetrate agentemulsifiersdevelopers etc. product series. The product performance complied with the specification and requirements of People Republic of China aerospace industry standard HB7681-2000 and US aerospace material specification AMS 2644E standard. The Index performance of some product peers

The Fluorescene Penetrant Agent Manufacture and Its ... · The manufactured fluorescent Penetrant agent performance complied with AMS 2644E ... Necessity and method of fluorescence

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17th World Conference on Nondestructive Testing, 25-28 Oct 2008, Shanghai, China

The Fluorescence Penetrant Agent Manufacture and Its

Wastewater Treatment

Zhenwang LIN 1 Zhenlu CHEN 1 Dongsheng LI 2 Jiangpai LI 3 Zhonglin CHEN 1 1Xiamen Jimei Xincheng NDT Manage Department

Rm.103,No.13,Fangzhi Road,Xinglin,Jimei District,Xiamen 361022, China Tel:86-592-5287678.Fax:86-592-6259989

E-Mail : [email protected]; E-Mail :[email protected] 2Honeywell TAECO Aerospace (Xiamen) Co.,Ltd , Xiamen, China

E-Mail :[email protected] 3Xiamen Airline Company Limited, Xiamen, China

Abstract

The author had spent decades in theoretical research and experiments in manufacturing water washable types and post emulsifiable fluorescence penetration

agent、emulsifiers、developers of various types etc. Thus the performance of this product

complied with the specification and requirements of People Republic of China aerospace industry standard HB7681-2000 and US aerospace material specification AMS 2644E standard. The Index performance of some product peers excelled and achieved international standards compared with similar product types. The author researched and explored the product in wastewater treatment with fluorescence penetration test process. By separation of oil from water and emulsion breakage and then finally achieving transparency and clear of the water. The wastewater of C O DCr value ranged from 10000 to 20000. After primary treatment, the clear water of C O DCr value reduced between 50 to 300. Whereby achieving an environmental protection level 3 effluent standards. The waste oil can be further reused optimized by further treatment.

Key word: fluorescence penetrant agent; performance; wastewater treatment; resource recovery

1. Introduction

The author had written several thesis related to penetrate topics(1)(2)(3)and

conducted laboratory experiments and theoretical researches for decades and had researched and manufactured water washable types and post emulsifiable types

fluorescence penetrate agent、emulsifiers、developers etc. product series. The product

performance complied with the specification and requirements of People Republic of China aerospace industry standard HB7681-2000 and US aerospace material specification AMS 2644E standard. The Index performance of some product peers

- 2 -

excelled and achieved international standards compared with similar product types. The author researched and explored the product in wastewater treatment with fluorescence penetration test process. By separation of oil from water and emulsion breakage and oil removal, oxidation mixed coagulant adsorption and filtration process and then finally achieving transparency and clear of water. Through separation of oil and water then emulsion breaking to removing oil ,oxidation degration, and filtration so as to achieve clear and transparency in the water. Whereby achieving an environmental protection level 3 effluent standards.

2. Fluorescence Penetrant agent research and manufacture: 2.1. Fluorescence Penetrant agent manufacture reference materials and test block

US Magnaflux Company :ZL-60D(fluorescence water washable type level 2) 、

ZL-67(fluorescence water washable type level 3) 、ZL-56(fluorescence water washable

type level 4).Germany Ardrox : 985-P13 (fluorescence post emulsifiable type level

3)ZL-27A(fluorescence post emulsifiable type level 3) and US Met-L-Chek:

FP-92B(fluorescence water washable type level 2) 、 FP-923B(fluorescence water

washable type level 3) 、FP-95A(fluorescence post emulsifiable type level 3) 、

FP-97A(fluorescence post emulsifiable type level 4) . E-58D emulsifier、 D-72A

developer which optimized the five spots type (twin block test) from US Sherwin Company and engaged into similar experiments for contrasting purposes.

2.2. Contents of experiments and results

Having conducting researches and manufacturing samples of water washable type and post emulsifiable type fluorescence Penetrant agent and the results reflected similar effects regardless in speedy removal, background removal, crack spots fluorescence brightness were almost equivalent in contrasted with other US samples as well as experiment in working conditions. The products were odour-free, close cup flash point

>93℃. Penetrant agent would not solidified in freezing temperature of below 0℃.

Corrosion test, water tolerance(method A only), emulsifier test, developer test etc. too

complied with with with with specifications and requirements. Detailed contents as shown in table 1-5:

Table.1 Fluorescence water washable type level 2

No Design-

tion Character

Specific Gravity

Freezing point

Viscosity Flash Point

Water

Tolerance

1 FA-2-1 Yellow-green

liquid 0.925 <0℃ 12cst >93℃ >5%

- 3 -

2 FA-2-2 Yellow-green

liquid 0.937 <0℃ 12.9cst >93℃ >5%

Removability and Sensitivity Contrast Test Corrosion Test

No.

Reference

Material Reference

Block Wash

Speed

Remove

Back-

ground

Crack spot

Fluorescent

Brightness

Al

Alloy

Mg

Alloy

Steel

1 Mag.ZL60D Sher.Dt.ww Equal Equal Equal Acc Acc Acc

2 Mag.ZL60D Sher.Dt.ww Equal Equal Equal Acc Acc Acc

Table 2 Fluorescence water washable type level 3

No Design-

tion Character

Specific

Gravity

Freezing

point Viscosity

Flash

Point

Water

Tolerance

1 FA-3-1 Yellow-green liquid 0.956 <0℃ 13cst >93℃ >5%

2 FA-3-2 Yellow-green liquid 0.97 <0℃ 16.2cst >93℃ >5%

Removability and Sensitivity Contrast Test Corrosion Test

No.

Reference

Material

Reference

Block

Wash

Spee

d

Remove

Background

Crack spot

Fluorescent

Brightness

Al

Alloy

Mg

Alloy

Steel

1 Met-L.923B Sher.Dt.ww Equal Equal Equal Acc Acc Acc

2 Met-L.923B Sher.Dt.ww Equal Equal Equal Acc Acc Acc

Table 3. Fluorescence water washable type level 4

No Design-

tion Character

Specific

Gravity

Freezing

point Viscosity

Flash

Point

Water

Tolerance

1 FA-4-1 Yellow-green

liquid 0.94 <0℃ 14cst >93℃ >5%

2 FA-4-2 Yellow-green

liquid 0.99 <0℃ 16.2cst >93℃ >5%

Removability and Sensitivity Contrast Test Corrosion Test

No Reference

Material

Reference

Block

Wash

Speed

Remove

Back-

ground

Crack spot

Fluorescent

Brightness

Al

Alloy

Mg

Alloy

Steel

1 Mag.ZL56 Sher.Dt.ww Equal Equal Equal Acc Acc Acc

2 Mag.ZL56 Sher.Dt.ww Equal Equal Equal Acc Acc Acc

Table 4. Fluorescence post emulsifiable type level 3 (hydrophilic)

No Design- Character Specific Freezing Viscosity Flash Emulsi-

- 4 -

tion Gravity point Point fier

1 FD-3-1 Yellow-green liquid

0.94 <0℃ 6.8cst >93℃ E1

2 FA-3-2 Yellow-green liquid

0.98 <0℃ 9.7cst >93℃ E1

Removability and Sensitivity Contrast Test Corrosion Test

No Reference

Material

Reference

Block

Wash

Speed

Remove

Back-

ground

Crack spot

Fluorescent

Brightness

Al

Alloy

Mg

Alloy

Steel

1 Ard.985-P13 Sher.Dt.PE Equal Equal ≥985-P13

Acc Acc Acc

2 Ard.985-P13 Sher.Dt.PE Equal Equal ≥985-P13

Acc Acc Acc

Table 5. Fluorescence post emulsifiable type level 4 (hydrophilic)

No Design-

tion Character

Specific

Gravity

Freezing

point Viscosity

Flash

Point

Emulsi-

fier

1 FD-4-1 Yellow-green liq. 0.955 <0℃

7.6cst >93℃

E1

2 FA-4-2 Yellow-green liq. 0.98 <0℃

9.8cst >93℃

E1

Removability and Sensitivity Contrast Test Corrosion Test

No Reference

Material

Reference

Block

Wash

Speed

Remove

Back-

ground

Crack spot

Fluorescent

Brightness

Al

Alloy

Mg

Alloy

Steel

1 Met.-L.97A Sher.Dt.PE Equal Equal >97A

Acc Acc Acc

2 Met.-L.97A Sher.Dt.PE Equal Equal >97A

Acc Acc Acc

2.3. Compare Picture: A comparison between the researched product and US AFRL

qualfied product of similar types in Penetrant agent removability and sensitivity (twin block test). Referred to Picture 1~4.

2.4. Emulsifier E1: hydrophilic type. Rose red aqueous solution. Concentration level of

20%%%%.

2.5. Developer D1: Dry powder. Accumulation density 0.15. Developer did not contain

asbestos.

- 5 -

Picture 1: ZL-67 & FA-3-1 Picture 2: FA-4-1 & ZL-56

Picture 3: FD-3-1 &ARD.985-P13 Picture 4: FD-4-1 & FP-97A

2.6. Conclusion

- 6 -

The manufactured fluorescent Penetrant agent performance complied with AMS 2644E specifications and requirements. In comparison with the US AFRL qualified products, by optimizing twin block test had shown that the performance was fundamentally equivalent. However the manufactured fluorescence water washable of

type level 3、4 water- proof had achieved equivalent or higher sensitivity level in

comparison with its peer products of international standards. The manufactured

fluorescence post emulsifiable of type level 3、4 crack spot fluorescent brightness also

achieved equivalent or higher contrasting levels in comparison with its peer products of international standards.

3. Fluorescent Penetrant agent wastewaterwastewaterwastewaterwastewater treatment

3.1.: Necessity and method of fluorescence penetrant agent wastewaterastewaterastewaterastewater treatment:

As you know that application of water washable types and post emulsifiable types fluorescence Penetrant agent onto work piece or spare-parts to conduct PT check and large volume of organic waste water will be produced during the removal process in PT

check (included water wash、prewash、post emulsifiable water wash and other removal

treatment). Hence the organic waste water contained oil, organic solvent, surfactants, organic dye and etc which resulted aqueous emulsion, fluorescence pollution, oil pollution, poison and other hazards in the water. C O DCr value ranged between 10000 to 20000 do not comply with the environmental protection effluent standards and requirements. The method for the modernized organic waste water treatment mainly (4)

degraded active dirt particles: Activated sludge microbiological degration treat method; Chemical oxidation degration treatment method. The author also conducted researches

and adopted a swift, simplified Fenton Reagent (H2O2+FeSO4•7 H2O ) chemical

oxidation degration method to degrade fluorescence wastewater and washable types of waste water and post emulsifiable types of waste water were to be treated separately. Therefore it provided referencing of experimentations for conducting a large scale treatment of fluorescence wastewater.

3.2. Procedures for Wastewater treatment:

Waste water→separating oil from water→heating & breaking emulsion and remove oil→low dose Fenton Reagent oxidation degration→coagulate adsorption→filter→clear water

The clarity and transparency of water after treatment. Originally, the C O D Cr value for

wastewater is ranged from 10000 to 20000.After primary treatment, the C O D Cr value for clear water was reduced between 50 to 300 which attained an environmental

- 7 -

protection level 3 effluent standard.

3.3. Wastewater treatment method and results

3.3.1.Low dose Fenton Reagent(H2O2++++FeSO4•7H2O) oxidation degration method:

Sampled 100 ml of wastewater, applied heat temperature till 70~80℃ then stirred and

add small amount of breaking emulsifiers. Then remove the upper layer of the floated oil and filtered the precipitate at the bottom layer. Add 0.25ml 1:4 H2SO4 solution to liquid.

Adjust PH level for liquid =3. Add 0.08g FeSO4•7 H2O , continue heating and stirred,

maintained temperature at 70~80℃. Slowly dripped about 30% of H2O2.. Hydrogen

peroxide consumption at 0.8ml~1.8ml, treatment of solution in accordance of high/low in

the C O D Cr value.... Reaction: Continue heating, stirred for 15 min. The treated solution

changed to transparent from corrosive liquid which resulted termination of reaction. Then

add coagulant 0.1g FeSO4•7 H2O [or Al2(SO4)3] and 0.2g CaO. Stirred for 1 min and it

resulted precipitation of brown flocculation. Then leave it for precipitate. Proceed to filtration while in hot temperature .So as to attain clear and transparent water

Remark: Wastewater of C O D Cr value which were higher, exceeded content of surfactant, achieved stability, C O D Cr value may not achieved effluent standard requirement during the first degration but repeated application of oxidation degration and coagulate adsorption treatment until it complied to the environmental protection effluent standards and requirement.

3.3.2. C O D Cr value sheet for Fluorescent pentrant wastewater treatment

- 8 -

3.3.3. Before and after treatment of wastewater: See Picture 5, 6

Picture 5: Treatment of Yellow-green color Picture 6: Treatment of Rose-red color wastewater wastewater

3.4. Conclusion and existing problem: (1) Compare with Activated sludge microbiological degration treatment method, the low

dose Fenton reagent oxidation degration and coagulate adsorption treated the fluorescent Penetrant wastewater, advantages for chemical reaction which processed

CODCr

Fenton Reagent Waste water type

Charcters Stability Original

waste

water

Separate

oil from

water 1st

degration

2nd

degration

Level 1,2 Yellow-green

Turbid liquid

Motionless

24 hour

lamination

~10000 ~2500 ~190-170

Clear water

Wa

ter

wa

sh ty

pe

Level 3,4 Yellow-green

Turbid liquid

No

lamination ~10000 ─

~2000

Clear Water

<<<<100-200

Clear Water

prewash Yellow-green

Turbid liquid

Easy

lamination ~20000 190~600

~50-190

Clear Water ─

Post emul.

water wash

Rose-red

liquid

No

lamination ~10000 ─ ~3000

Clear Water

~1000

Clear Water

Pos

t em

ulsi

fiabl

e ty

pe

Prewash &

Post emul.

water wash

Yellow-red

Turbid liquid

Easy

lamination ~20000 ~7000

~2000

Clear Water

~300

Clear Water

- 9 -

the wastewater: speedy reaction, short process flow, equipment easy to operate and etc.

(2) Some post emulsifiable which cleansed wastewater that adopted separation of oil from water which were not required to undergo further treatment. CODCr value lower than 300 which were not required for treatment and can be directly effluent. If a number of fluorescent wastewater presented content of surfactant and CODCr value

was higher showed that greater stability, one-time degration of CODCr value will not meet the effluent specification and requirements. So repeatedly degrading of oxidation process will consume greater amount of oxidizing agent. The technology must be further upgraded and researched in addition of adaptation of other degration method for assistance.

(3) Wastewater for washable type and post emulsifiable fluorescence type shall be

treated separately, separate oil from water, further by emulsion breaking shall be beneficial as it reduce the consumption of oxidation agent and related treatment cost.

(4) Separated the waste oil shall be further do resource recovery or usage for fuel

burning.

Reference:

(1)Lin Zhenwang “Metallic Penetrant testing mechanism and Penetrant agent

molecular structure”. 7th Asian-Pacific Conference on NDT. 1993 Shanghai China. p.728

(2)Lin Zhenwang “Surfactants as Applied to Penetrant Test”.US “Materials

Evaluation”. Oct.2001 p.1205 (3)Lin Zhenwang “Micro emulsion Penetrant agent manufacture” 8th China NDT

Conference. 2003 Suzhou China (4)Li Yafong “Practical Waste Water Treat Technique“. China Chemical industrial

publishing house 2007