‘Accessed by WOODSIDE ENERGY LTD on 19 Oct 2001 AS 1627.5—1994 Australian Standard® Metal finishing—Preparation and pretreatment of surfaces Part 5: Pickling, descaling and oxide removal‘Accessed by WOODSIDE ENERGY LTD on 19 Oct 2001 This Australian Standard was prepared by Committee MT/9, Metal Finishing. Tt was approved on behalf of the Council of Standards Australia on 7 March 1994 and published on 16 May 1994, ‘The following interests are represented on Committee MI/9: Aluminium Development Council Australasian Institute of Metal Finis ng Australian Chamber of Commerce and Industry Department of Defence ‘Metal Trades Industry Association of Australia Royal Australian Chemical Institute ‘Telecom Australia University of Queensland Additional interests participating in preparation of Standard: AUSTROADS Blast Cleaning and Coating Association of Australia Review of Ausralin Standards. To tap abreast of progress in industry, Australian Standards are subject {periodic review and are hapt uptodate bythe iwc of amendments or new editons a necesary Ie Unportant therefore that Standards srs enate that they are In possession of the latest ection, and ens ‘amendments tere Full details of all Australian Standands and laced publications will be found in dhe Standards Australia logue of Publications: tis information supplemented each montk by the magacine ‘The Australien Standard’, hick subsenbing members receive, and which ives detaile of new publications, new etons fad amendments, and of withdrawn Standards Suggestions for improvements te Australian Standards, addressed ro the head ofie of Standards Australia, fre welcomed. Nowfieation of any inaccuracy or ambigaty foal an Ausraan Standard should be made ‘sikoat delay inorder thatthe mater may be investigated ond dppreprate act taken. This Standard was issued in draft form for comment as DR 92232.‘Acceesed by WOODSIDE ENERGY LTD on 19 Oct 2001 AS 1627.5—1994 Australian Standard® Metal finishing—Preparation and pretreatment of surfaces Part 5: Pickling, descaling and oxide removal PUBLISHED BY STANDARDS AUSTRALIA (STANDARDS ASSOCIATION OF AUSTRALIA) } THE CRESCENT, HOMEBUSH, NSW 2140 ISBN 0 7262 8852 7‘Acoessed by WOODSIDE ENERGY LTD on 19 Oct 2001 AS 10275—1998, 2 PREFACE This Standard was prepared under the direction of the Multitechnics Standards Policy Board by the Standards Australia Committee on Metal Finishing to supersede AS 1627.5—1975, Metal finishing—Preparation and pretreatment of surfaces, Patt 5: Pickling steel surfaces. It has been expanded to include methods for the preparation of other metals, in addition to steel, and now contains information on hydrogen ‘embrittlement relief and stress relief of metals. This Standard is one of a series of Standards covering the preparation and pretreatment of metal surfaces used in metal finishing, Others in the series are as follows AS 1627.0 Part 0: Method selection guide for preparation and pretreatment of steel surfaces 1627.1 Part 1: Cleaning using liquid solvents and alkaline solutions 1627.2 Part: Power tool cleaning 1627.3 Part3: Flame descaling 1627.4 Part 4: Abrasive blast cleaning 1627.6 Part 6: Chemical conversion treatment of metals 1627.7 Part 7: Hand tool cleaning of metal surfaces 1627.9 Part 9: Pictorial surface preparation standards for painting steel surfaces 1627.10 Part 10: Cleaning and preparation of metal surfaces using acid solutions (non- immersion) ‘The terms ‘normative’ and ‘informative’ have been used in this Standard to define the application of the appendix to which they apply. 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This polcy miy be vane by Stancards Ausralia3t Sry Woe,‘Accessed by WOODSIDE ENERGY LTD on 19 Oct 2001 CONTENTS FOREWORD «2.2.0.6. cece cece e cee ee eee ee ete SECTION 1 SCOPE AND GENERAL Ld 12 13 14 15 16 SCOPE ....... REFERENCED DOCUMENTS DEFINITIONS SURFACE CONDITION REQUIREMENTS AFTER TREATMENT SAFETY PRECAUTIONS .. : DISPOSAL OF WASTE SOLUTIONS é SECTION 2 PROCEDURES 24 2.2 2.3 2b 25 2.6 27 2.8 2.9 GENERAL, EQUIPMENT PICKLING AND DESCALING METHODS FOR FERROUS MATERIALS CLEANING AND OXIDE REMOVAL FROM ALUMINIUM AND ALUMINIUM ALLOYS CLEANING AND OXIDE REMOVAL FROM COPPER AND COPPER ALLOYS. CLEANING AND OXIDE REMOVAL FROM ZINC AND. ZINC ALLOYS . CLEANING AND OXIDE REMOVAL FROM NICKEL AND NICKEL ALLOYS . RINSING AND DRYING FINAL CLEANING . 2.10 CORROSION PROTECTION APPENDICES A B c PURCHASING GUIDELINES . WET SMUT TEST ADVICE ON HEAT TREATMENT OF STEEL FOR RELIEF OF HYDROGEN EMBRITILEMENT AND STRESS AS 162751994 - 10 u 212 B 4 4 . 1s . 16 7[Accessed by WOODSIDE ENERGY LTD on 19 Oct 2001 AS 1627.5—1994 4 FOREWORD Pickling is used for the complete removal of scale, metallic oxides or other contaminants from metal surfaces prior to the application of a suitable protective coating. Tt is used as an alternative to mechanical methods such a5 abrasive blast cleaning. The surface produced by pickling is generally smooth, and may not be suitable for the application of some coatings, e.g. inorganic zinc and high-build epoxy coatings, or for metal spray coatings. The use of corrosion inhibitors in rinse solutions to prevent early rusting of a pickled surface may also cause incompatibility with subsequent coatings. Coating manufacturers or suppliers should be consulted before the application of coating systems to pickled surfaces is carried out The two most common acids used for pickling are sulfuric acid and hydrochloric acid. With increasing enforcement of anti-pollution regulations, the popularity of the cheaper sulfuric acid is declining, as hydrochloric acid is more easily recovered in acid regeneration plants and hence is favoured for continuous pickling installations. Hydrochloric acid is also more practicable for batch pickling because the high heat of reaction reduces the amount of external heating necessary. It also dissolves scale faster than sulfuric acid, Acid fuming, often cited as a major deterrent to hydrochloric acid pickling, can be effectively controlled by adhering to correct operating procedures, Other acids, such as phosphoric, nitric, hydrofluoric, citric and sulfamic, are used for special purposes. An inhibitor should always be used with any acid to prevent excessive attack on the base metal during pickling, Special finishing precautions, including fresh water rinsing, are necessary to remove residues of unreacted acid. Final rinses containing dilute phosphoric or chromic acid are often used to temporarily passivate the pickled surface. Pickled steel, like blast-cleaned steel, should be painted as soon as possible after cleaning and drying, During the design of fabricated steel, special consideration should be given to the elimination of pockets or crevices which can trap acid during pickling.[Acoessed by WOODSIDE ENERGY LTD on 19 Oct 2001 5 AS 16275-1994 STANDARDS AUSTRALIA Australian Standard Metal finishing—Preparation and pretreatment of surfaces Part 5: Pickling, descaling and oxide removal SECTION | SCOPE AND GENERAL LI SCOPE This Standard sets out procedures for preparing metal surfaces by immersion, or by other means, employing chemical solutions to remove oxidation products (scale), corrosion products and related foreign materials. It includes acid pickling and alkaline descaling methods for the following materials: (a) Steels: (b) Cast iron. (©) Aluminium and aluminium alloys, (@ Copper and copper alloy (©) Zine and zinc alloys. (f) Nickel and nicket alloys. NOTE: Advice and recommendations on information to be supplied by the purchaser at the time of enquiry or order are contained in Appendix A. 1.2. REFERENCED DOCUMENTS The following documents are referred to in this Standard: AS 1319 Safety signs for the occupational environment 1337 Bye protectors for industrial opplications 1470 Health and safety at work—Principles and practices 1627 Metal finishing—Preparation and pretreatment of surfaces 1627.1 Part 1: Cleaning using liquid solvents and alkaline solutions 1627.2 Part 2; Power tool cleaning ITIS Selection, use and maintenance of respiratory protective devices 1716 Respiratory protective devices 1874 Aluminium and aluminium alloys —Ingots and castings 2161 Industrial safety gloves and mittens (excluding electrical and medical gloves) 2453 Electroplated coatings of chromium for engineering applications 2848 Aluminium and aluminium alloys—Compositions and designations 2848.1 Part 1: Wrought products ASTM A380. Practice for cleaning and descaling stainless steel parts, equipment, and systems coPyRIGHT‘Accessed by WOODSIDE ENERGY LTD on 19 Ort 2001 AS 16275 —1994 6 1.3. DEFINITIONS For the purpose of this Standard, the definitions below apply. 1.3.1 Alkaline desealing—the process of descaling a metal by immersion in a hot alkaline solution. 1.3.2. Electrolytic desealing—the process of descaling a metal by making it an electrode in a bath containing a suitable electrolyte. 1.33 Hydrogen embrittlement—a loss of ductility in metals caused by absorption of hydrogen. 1.3.4 Inhibitor—a substance added to a solution to inhibit or prevent a chemical electrochemical reaction. 1.3.5 Pickling—a treatment for the removal of scale or corrosion products from a metal surface by immersion in a solution, usually acid. 1.3.6 Seale—the heavy oxide layer formed on the surface of metals during heat treatment or hot working, 1.3.7 Smut—a reaction product sometimes left on the surface of a metal after a pickling or an etching operation. 1.4 SURFACE CONDITION REQUIREMENTS AFTER TREATMENT 14.1 General The surface of materials treated in accordance with procedures in Section 2 of this Standard shall be free of scale, metallic oxides, grease, dirt or other surface contamination that will affect the appearance, further processing or end use of the product. Any inbibitive coating shall be firmly adherent to the underlying metal. Castings shall be free from foundry sand. 1.4.2 Removal of smut deposits During pickling, some alloys, c.g. aluminium alloys containing copper, iron, manganese or silicon, develop a grey to black deposit on the surface which can have a detrimental effect on the adhesion and appearance of subsequent coatings. Carbon smuts may also occur on steel and nickel alloys. The removal of such smut deposits can be achieved by treatment with acid mixtures or proprietary desmutting solutions. A test for determining the presence of smut is given in Appendix B. 13 SAFETY PRECAUTIONS 15.1 General For requirements for effluent disposal, ventilation, protective clothing and safety equipment, reference shall be made to the relevant regulatory authority Personnel who carry out metal finishing treatments shall be instructed in safe working methods (see AS 1470) 1.5.2. Health hazards Operators shall be aware of the health hazards involved in the handling of the various acids, inhibitors or additives referred to in this Standard. If the user is unfamiliar with the hazards which may be associated with any material or process, consultation shall be carried out with the supplier of the material or with chemical safety experts, 1.5.3 Handling solutions Personnel shall be instructed in the s solutions. fe handling of It is important that the addition of concentrated acid to cold water or to cold dilute acid is carried out very slowly and with continuous stirring. Water shall not be added to concentrated acid under any circumstances, due to the resultant violent boiling reaction and consequent splashing. WARNING: EXTREME CARE IS REQUIRED IN HANDLING HYDROFLUORIC ACID. IT IS ESSENTIAL THAT THE MANUFACTURER'S: INSTRUCTIONS BE FOLLOWED IMPLICITLY AS BURNS DUE TO CONTACT WITH THE ACID MAY BE APPARENT ONLY AFTER SEVERAL HOURS. copyaiaHt‘Accessed by WOODSIDE ENERGY LTO on 19 Oct 2001 7 AS 162781995 154 Protective clothing Suitable safety clothing including face and eye protection devices, rubber aprons, boots and gloves shall be worn where hazards resulting from splashing may occur (see AS 1337 and AS 2161). 1.5.5 Ventilation Adequate ventilation shall be provided for all pickling operations to protect the health of operators and to minimize concentrations of hydrogen gas and acid fume in confined spaces. Acid spray can be reduced by blanketing the surface of the bath with foam, plastic balls or other means. 1.5.6 Respiratory protection Approved respiratory protection devices shall be provided where fuming hazards exist (see AS I7I5 and AS 1716). 1.5.7 Safety signs Safety signs complying with AS 1319 shall be prominently displayed in the working area, 1.5.8 Washing facilities Sufficient washing facilities shall be provided in case of accidental splash or spillage of solutions which may burn, irritate or otherwise be harmful when in contact with the skin. The equipment shall include an eyewash facility of appropriate type in each room where corrosive substances are handled. It should comprise a permanently-fixed acrated cycwash system which can be operated without using hands. The equipment shall also include at least one safety shower of an appropriate type located not more than 10m travel distance from the source of corrosive liquid 1.6 DISPOSAL OF WASTE SOLUTIONS The local waste disposal authority, the environment protection authority and the health department, as appropriate, shall always be consulted on the acceptability of the proposed method of disposal. Advice may also be provided by the chemical companies supplying the products. NOTE: It may be appropriate to employ the services of a licensed trade waste disposal contractor for the disposal of waste solutions. COPYRIGHT‘Accessed by WOODSIDE ENERGY LTD on 19 Cet 2001 AS 16275-1988 ® SECTION 2 PROCEDURES 24 GENERAL Most methods of preparing metal surfaces require immersion of the metal in a bath containing an aqueous solution of one or more reagents. The treatment time will depend on the operating conditions and the nature of the work. The time required to pickle a particular product is best determined by trial. Movement of the metal in the bath, agitation of the solution, or spray treatment can be used to increase the rate of processing and to achieve surface uniformity. NOTE: High strength steels are susceptible to hydrogen embrittlement when subjected to some metal finishing operations. Advice on heat treatment procedures to relieve hydrogen ‘embrittlement is given in Appendix C. 2.2 EQUIPMENT The cleaning process, whether batch or continuous, usually requires fan array of tanks, the size of which depends on the dimensions of the material being pickled. Ail storage, descaling and rinse tanks, and supply lines and valves are required to be constructed from, or lined with, materials resistant to the chemical solutions being used. 2.3. PICKLING AND DESCALING METHODS FOR FERROUS MATERIALS. 2.3.1 Preliminary cleaning Weld spatter and slag, if present, shall be removed prior to pickling Solvent or alkaline cleaning and, if necessary, mechanical methods of preparation shail be used initially to remove deposits of oil, grease, dirt or other matter which are not removable by pickling (see AS 1627.1 and AS 1627.2). Small quantities of such matter may be removed by the pickling procedures, provided that no detrimental residues remain to reduce the efficiency of the pickling solutions, 2.3.2 Piekling of low carbon steel Solutions suitable for the pickling of low carbon steel include sulfuric acid, hydrochloric acid, phosphoric acid, citric acid and sodium hydroxide (alkaline descaling). Recommended solution concentrations, solution temperatures and general control procedures are given in Table 2.1 For plain carbon steels, the addition of an inhibitor to the solution is recommended to retard chemical attack on the base metal and to limit hydrogen absorption. ‘Typical inhibitor concentrations are given in Table 2.1. As most inhibitors in use are proprietary lines, the actual type and concentration of the inhibitor should be in accordance with the ‘manufacturer's recommendations. 23.3 Pickling of cast iron and cast steel Solutions containing a mixture of sulfuric and hydrofluoric acids are generally used for pickling cast iron and cast steel. The concentration of each acid will depend on whether the prime purpose of the pickling process is for sand removal or for scale removal. ‘Typical concentrations are given in Table 2.1. Inhibitors or wetting agents are not normally used for these applications. 2.3.4 Pickling of stainless steel Stainless steels may be pickled by immersion in a nitricMydrofluoric acid mixture at the concentration levels indicated in Table 2.1. Normally, no inhibitor is used as more chemical activity is required to remove the oxide scale than in the case of low carbon steels. Further information on acid descaling and cleaning of stainless steel is contained in ASTM A380. coPyRIGHT‘Accessed by WOODSIDE ENERGY LTD on 19 Oct 2001 ° AS 162751998 TABLE 21 PICKLING AND DESCALING METHODS FOR FERROUS METALS ‘i ‘Typical operating conditions (Note 1) | Tron Typical acai Piekin tE|tecrsne concentration | inhibitor solution 7 Umit ‘concentration Concentration | ‘Temperature ar nae Sulfuric acid (3% 10% WW [60°C w AOC | Discard solution [0.1% 10 03% (py 1.84 g/mL) st 6% to 8% | addition based iron content Jon mass of pure #80, Hydrochloric acid | 16% to 40% YT nbient 1 50°C [Discard solution [0.1% to 02% (py 1-16 gml) (oe 3) 10% iron ation ‘hased content on total solution {Phosphoric acid [5.5% to 17% VW | Ambient © 95°C | Discard solution [0.05% addition Stee! (py 1.69 pm at 6% 19 8% [based on total (low iron content| solution carbon} Citric acid [3a to $8 cine acid [85°C to 95°C = (0.05% to 0.10% a) addition based on total solution Sodium hydroxide [10% NaOH (mim) ]90°C 10 95°C 7 = Cast iron [Sulfuric acid (3% HSOAS%HF [65°C 10 85°C for and (py 184 gimLy |v sand removal cast steel | hydrofivoric acid - = (zm 1.16 g/mL) | 7% HS0.43% HF |$0°C w 85°C for 2 Suitable inhi 2.4 CLEANING AND OXIDE REMOVAL FROM ALUMI ALUMINIUM ALLOYS: 2.4.1 General Aluminium and aluminium alloys require scale and oxide removal prior to processes such as welding, painting, conventional coating, bright dipping and anodizing. Acid solutions acting as deoxidizers are used for the selective removal of aluminium oxide films and coatings. mixture iw scale removal ‘Stainless 8% 10 12% nbient Discard solution stoel HHNO,42% to 4% HF |temperatore Jat 5% iron hydrofluoric acid | VV [maximum | content 7 (Pw 116 gimL) immersion time mixture 3 min) NOTES: The selection of acid concentration and solution temperature will depend on the section being pickled, the type of scale, or whether a batch or a continuous process is utilize. iors include natural and synthetic organic compounds and some inorganic compounds Proprietary lines should be used in accordance with the manufactore’s recommendations 3 The normal operating temperature (40°C) for hydrochloric acid pickling is reached through heat generated by the pickling reaction. At a tomperature of SO°C, the speed of reaction is greatly increased causing high evaporation losses. [UM AND The most widely used method for cleaning aluminium and aluminium alloys employs alkaline solutions (see AS 1627.1); however, some acid cleaning processes are also used. Typical acid mixtures include chromic/sulfuric, —_phosphori nitricfhydrofluoric although some proprietary non-etching acid cleaners are also available. hromic and CoPvRIGHTAcoeseed by WOODSIDE ENERGY LTD on 18 Get 2001 As 162751904 0 24.2 Alloy limitations Aluminium alloys containing more than 0.5% copper and 1% silicon are usually not amenable to acid cleaning. These alloys comprise some of the 2000 and 4000 Series (wrought alloys) and the 300 and 400 Series (casting alloys) specified in AS 2848.1 and AS 1874, respectively, and are normally cleaned by mechanical methods. NOTE: Alloys with a copper content grester than 0.5% can be treated with special formulations. When proprietary processes are used, the manufacturer's advice should be sought concerning the suitability for a particular alloy. 2.43 Preliminary cleaning Articles which have been heat treated in a salt bath or which have been welded should be washed until all soluble salts or welding flux have been removed. The practice of quenching heated articles in near boiling water, or the use of alternate hot and cold water quenching will often assist in the removal of salts from recesses. Articles which are contaminated with oil or grease should be degreased with liquid solvent in accordance with AS 1627.1, Loose soil and oxide can be removed by light mechanical brushing with a non-metallic abrasive. 24.4 Seale and oxide removal Typical acid solution compositions, concentrations and operating conditions for the removal of scale and oxide deposits from aluminium surfaces are as follows: (8) Hydrofluorie sid (0 1.69 ght HE)... 10% VV Nitric acid (Py 1.42 g/mL)....... 20... 10% VV Water remainder Temperature... .... bees eens 25°C to 40°C Immersion time I min to 5 min (©) Sulfuric acid (Pip 1.84 g/mL)... 0.0.2... 15% WV Sodium dichromate or chromic acid ...... 7.5% m/V or 5% m/V respectively Water remainder ‘Temperature + 60°C to 70°C Immersion time .. - min to 2 min (©) Phosphoric acid (Pq) 1.69 g/mL) cee SHV Chromic acid 15% mV Water cere oe eee ses. remainder Temperature sees 45°C to 65°C Immersion time... 02.00 ....0e0e. e+ Emin to 5 min Where immersion processes are impractical, proprietary acid solutions may be applied by brushing or swabbing. In such cases the manufacturer's instructions should be carefully followed, applying the (diluted) solution to the metal surface with a brush or mop and moving the applicator over the soiled or oxidized areas until the soil or oxide is removed, 24.5 Rinsing All excess acid shall be removed by rinsing with clean water, taking care to contain residual chemicals and the rinses for disposal treatment (see Clause 2.8). NOTE: Where thickening agents are incorporated in the solution formulation, special care is needed to ensure their complete removal. 25 CLEANING AND OXIDE REMOVAL FROM COPPER AND COPPER ALLOYS 2.5.1 General In many cases, mechanical preparation is the only pretreatment applied to copper and copper alloys. Acid pickling is necessary only in those cases where heavy scale (e.g. from heat treatment) is present. When this occurs, sulfuric or hydrochloric acid is generally used. Sometimes no additional surface preparation is necessary to produce the desired finish, but heavily scaled material may require a ‘scale’ dip or bright dip after coPYRIGHT‘Accessed by WOODSIDE ENERGY {TD on 19 Oct 2001, " AS 10278—1904 pickling. Scale and bright-dip solutions for copper and copper alloys generally consist of sulfuric and nitric acids in varying proportions. Proprietary solutions using sulfuric acid and stabilized hydrogen peroxide are also available. The actual choice of the pickling medium depends on the metal/alloy composition and the type of oxide scale present, 2.5.2 Preliminary cleaning A completely dry article may be treated with organic solvents and then with an aqueous alkaline cleaner (see AS 1627.1). Wet articles should be processed directly into an alkaline cleaner of sufficient concentration to prevent oxidation. 2.5.3. Seale and oxide removal Typical acid solution compositions, concentrations and operating conditions for the removal of scale and oxide deposits from copper surfaces are as follows: (@) Sulfuric Acid (Po 1.84 g/mL) sees 4 to 15% WV Water... . cesses remainder ‘Temperature a 25°C to 50°C NOTE: The oxide film of copper and copper alloys with more than 85% copper contains high percentages of cuprous oxide (Cu,0) which is not easily removed by sulfuric acid, In this case it is desirable to add oxidizing agents to the solution. (©) Hydochlrie acid (Oy 116 gol)... 40% w SO V7 Water... 0. cose es neomainder Temperature... ee eee eee eens 25°C (©) Where a bright dip is required, the article should be immersed in a solution consisting of the following: Sulfuric acid (Py 1.84 g/mL) ....... 50% V/V Nitric acid (y 1.42 gimL)......... 25% V/V Sodium chloride or hydrochloric acid cece ees 0.1% mV Water sees s remainder Temperature... see. ee ees 25°C NOTES: This solution attacks copper-base alloys vigorously and is therefore not recommended for parts having thin sections or elose tolerances. 2. Efficient fume extraction is essential as the process results in the evolution of highly toxic fumes (a) Where chemical smoothing is required, the following solution and operating temperature may be used: Sulfuric acid (Py_ 1.84 g/mL) ....... 10% to 20% W/V Hydrogen peroxide (Px 1 13 gmt) ++ 3% 10 5% VV Water... . . remainder ‘Temperature, 20°C to 80°C Where immersion processes are impractical, proprietary acid solutions may be applied by brush, swab or mop until the soil and patina are removed. 2.5.4 Rinsing All excess acid shall be removed by rinsing with clean water, taking care to contain residual chemicals and the rinses for disposal treatment (see Clause 2.8). NOTE: Where thickening agents are incorporated in the solution formulation, special care is needed 10 ensure their complete removal. 2.6 CLEANING AND OXIDE REMOVAL FROM ZINC AND ZINC ALLOYS 2.6.1 General Acid cleaning is usually applicable to zinc diecastings, rolled zine and galvanized (including zinc/aluminium) surfaces. COPYRIGHT‘Acseesed by IMOODSIDE ENERGY LTD on 19 Oct 2001 AS 162781995 2 Zinc-based diecastings are characterized by a dense, fine-grained surface structure, and are frequently of a complex shape. They are sensitive to attack by caustic alkalis and, if electroplated, care is required to avoid prolonged contact with strong alkali cleaners to avoid blistering of the primary copper coating. Failure to achieve a proper cleaning cycle will result in the separation of this coating, usually through the formation of blisters. When the blistering is due to undercleaning, the back of a detached particle will have the characteristic copper colour, whereas if the article is overcleaned, the colour will be grey. Solutions are formulated for the cleaning, oxide removal and integral zinc phosphating of lightly oxidized surfaces but are not suitable for surfaces coated with ‘white rust’. ‘The resultant surface is suitable for the application of a chemical conversion coating or a wash primer or other suitable primer. When required, thickening agents may be added to assist in maintaining solution contact. NOTE: For new zine surfaces, acid cleaning and oxide removal are not required provided that suitable coatings are selected. 2.6.2 Preliminary cleaning Articles which are contaminated with oil or grease shall be degreased with liquid solvent in accordance with AS 1627.1. Loose soil and oxide can be removed by light mechanical brushing with a non-metallic abrasive. Precleaning for electroplating is usually carried out using a hot, inhibited and buffered alkaline soak cleaner (with or without prior solvent treatment), and sometimes with vapour or emulsion cleaning, depending on the extent of contamination to be removed. 2.6.3 Scale and oxide removal A typical solution composition and operating temperature for the removal of scale and oxide deposits from zinc surfaces is as follows: Sulfuric acid (Oy 1-84 gmL) ....... 0.25% 10 0.75% WV Water... ete remainder ‘Temperature 7 ambient Similar solution concentrations of hydrofluoric acid or a mixture of sulfuric acid and hydrofluoric acid are also used. Citric acid may be used for very mild acid dipping. Where immersion processes are impractical, proprietary acid solutions may be applied by brush, swab or mop until the soil and oxide are removed. When using a combination cleaning/phosphate formulation, the solution should be applied until a grey coating forms. NOTE: If it is necessary to electroclean the article cathodically, care is required to ensure that etching does not occur. 2.64 Rinsing All excess acid shall be removed by rinsing with clean water, taking care to contain residual chemicals and the rinses for disposal treatment (see Clause 2.8) NOTE: Where thickening agents are incorporated in the solution formulation, special care is needed to ensure their complete removal. 2.7 CLEANING AND OXIDE REMOVAL FROM NICKEL AND NICKEL ALLOYS. 2.7.1 General The treatment for nickel and its alloys varies with the type of alloy being treated 2.1.2 Preliminary cleaning Nickel alloys are cleaned satisfactorily by the use of vapour, solvent, emulsion, alkaline soak or spray degreasing 2.7.3. Final electrocleaning The removal of final traces of dirt, grease and oil is best accomplished by electrolytic cleaning, Anodic treatment is suitable provided that the oxide coating formed is removed in subsequent treatment steps. COPYRIGHT‘Accessed by WOODSIDE ENERGY LTD on 18 Oct 2001 5 AS 16275 —1995 2.7.4 Activation An activation procedure is necessary to ensure the adhesion of a metallic coating to the base metal. A mild etching treatment is suitable for highly finished surfaces, but may result in sacrificing maximum adhesion. The following processes may be used separately: (a) Etching by immersion Immerse the article for a maximum period of 1 min in the following solution at room temperature: Ferric chloride seen eee + 25% £0 30% m/v Hydrochloric acid (Pq) 1-16 g/mL) 15% t0 16% V/V (b) Anodic etch Etch the article anodically by using a current density of 2.15 kA/m* for 2 min and follow with a cathodic treatment for 2s to 3 s in a solution containing 15% V/V (150 mL/L) of sulfuric acid (1.84 g/mL) at 20°C to 25°C. s treatment is recommended for heavy deposits on nickel. Care is required with nickel-copper alloys which may cause copper deposition during the cathodic cycle (©) Nickel strike Where a simultaneous activating/plating procedure is desired, make the article anodic for 2 min, then cathodic for 6 min, using a current density of 320 A/m’, in the following solution held at a temperature of 20°C to 25°C: Nickel chloride ......... cece eee es 24% m/V Hydrochloric acid (Py) 1.16 g/ml.) 6.5% VV This treatment is preferred for decorative nickel plus chromium deposits. NOTE: Difficulty is sometimes experienced in achieving adhesion of electrodeposited nickel on nickel alloys which contain a high proportion of chromium because passive oxide films readily form on the surface. Before depositing the nickel it is necessary to apply a treatment which will remove and prevent the reformation of these films. Sueh nickel alloys should be treated in accordance with the conditions outlined in Item (c). 2.8 RINSING AND DRYING 28.1 Draining During pickling the article shall be supported in a manner which will minimize entrapment of the pickling solution, to facilitate draining. After removal from the pickling bath it shall be allowed to drain freely; the draining time shall be controlled to prevent drying before rinsing. 2.8.2 Rinsing Pickled material shall be rinsed promptly, particularly if the acid is hot, to prevent the film drying, as resulting residues will cause problems in the operations that follow. Therefore after draining, rinse the article by either water spraying or immersing in a bath of water for 0.5 min to I min. The rinse water may be heated to facilitate drying or to prevent distortion of light gauge items. Excessive build-up of the pickling solution in a rinse bath during successive batches of work shall be prevented by continually overflowing the bath with fresh water, or by regular dumping. Other methods such as single-stage or multi-stage counterflow rinsing can be used to minimize the consumption of water. The content of acid or alkaline carryover shall be checked by a similar method to that used to control the pickling bath. 2.8.3 Rinse additives To prevent early oxidation of the cleaned surface after pickling, it is desirable to add a passivating additive to the rinsing bath. If two or more rinse baths fare used, the passivating additive should be added to the final rinse bath. Typical additives include nitrites, nitrates, phosphates, chromates, carbonates, silicates, borates, and amines. 2.84 Drying After rinsing, the article shall be drained and dried in an oven, or by an air blast from which oil and water have been removed. Alternatively, the final rinse may bbe operated at elevated temperatures. The article shall not be allowed to remain wet in whole or part for prolonged periods. NOTE: During drying, ferrous materials may develop a slight rust stain which may discolour the work. This discolouration is not detrimental to the surface integrity of the material ‘COPYRIGHT‘Accessed by WOODSIDE ENERGY LTD on 19 Oct 2001 AS 1627-51994 i 2.9 FINAL CLEANING In the event of the surface becoming contaminated during the period between the pickling operation and the application of the protective coating, it shall be recleaned by repeating the necessary procedures specified in Clauses 2.3, 2.4, 2.5, 2.6 or 2.7. 2.10 CORROSION PROTECTION Aficr drying in accordance with Clause 2.8.4, the appropriate protective coating shall be applied to the metal surface before corrosion occurs. Any slight rust staining occurring during the drying of ferrous materials may be ignored; however, it is important that any powdery or loose rust dust present on the surface is removed. The protective coating selected shall, in all cases, be tolerant of the surface condition, It is preferable to apply the coating while the metal is still warm after drying. copyright‘Acoested by WOODSIDE ENERGY LTD on 19 Oct 2001, 15 AS 16275 —1994 APPENDIX A PURCHASING GUIDELINES (informative) AL GENERAL Australian Standards are intended to include the technical provisions necessary for relevant products, but do not purport to comprise all the necessary provisions of a contract. This Appendix contains advice and recommendations on the information to be supplied by the purchaser at the time of enquiry or order. Its aims are to avoid misunderstanding, and to result in the purchaser receiving satisfactory products and services. A2 INFORMATION TO BE SUPPLIED BY THE PURCHASER The purchaser should supply the following information at the time of enquity or order: (a) Details of the article to be treated and its material specification. {b) Method to be used, {c) Treatments required for welds and steel defects. if applicable, (a) Requirements for the prior removal of grease and oil. (c) Degree of cleanness required for the subsequent protective coating. (f) Maximum delay allowed before coating application (g) Nature of the coating. (bh) Quality contro! and inspection requirements. (@) Special requirements for particular site and weather conditions. (Requirement for hydrogen embrittlement relief after pickling, if applicable. (k) Reference to this Australian Standard, i.e. AS 1627.5. coPyRIGHTAs 1027 5— 1994 6 APPENDIX B WET SMUT TEST (Normative) B1 SCOPE This Appendix sets out a method for determining the presence of smut on a metal surface using wet wiping agents on a wet surface. B2 PRINCIPLE The wet metal surface is wiped with cloth or paper and then examined for the presence of obvious marking indicating disturbance of smut, B3 MATERIALS Lint-free cotton cloth or high-wet-strength paper. B4 PROCEDURE The procedure shall be as follows: (a) Apply the cloth or paper. previously wetted with water, to the wet metal surface with moderate finger pressure and traverse the surface for a length of approximately 100 mm. (b) Inspect the metal surface for a traverse mark. BS INTERPRETATION Any obvious mark produced on the wet metal surface indicates, disturbance of surface smut. NOTE: With certain alloys and surface treatments, some marking may be allowable. B6 TEST REPORT The test report shail include the following information: (a) Name of the testing authority. (b) Report number and date of issue. (©) The type of metal or alloy tested. (@) The test result, (©) Reference to this test method, i.e. Appendix B of AS 1627.5. ‘Accessed by WOODSIDE ENERGY LTD on 19 Oct 2001 ‘COPYRIGHTAccessed by WOODSIDE ENERGY LTD on 19 Cet 2001 ” AS 162781994 APPENDIX C ADVICE ON HEAT TREATMENT OF STEEL FOR RELIEF OF HYDROGEN EMBRITTLEMENT AND STRESS (informative) C1 INTRODUCTION Hydrogen embrittlement may be defined as a decrease in the ductility of a metal resulting from the absorption of atomic hydrogen. The metal finishing operations of pickling, electrocleaning, electroplating, acid treatment and chemical stripping provide conditions under which hydrogen can be introduced into the metal structure. This hydrogen can markedly lower the maximum stress that the metal component may endure before brittle failure occurs, irrespective of the method of application of the stress. ‘These effects are most noticeable in steels possessing high tensile strength (or equivalent high hardness), in components with a high intemal residual stress and in components operating at high stress levels. They have also been observed in a wide variety of other materials including nickel-based alloys and austenitic stainless steels. Hydrogen embrittlement rarely occurs in steels with tensile strength below 1000 MPa. The effects of hydrogen embrittlement can be minimized by heat treatment. Such heat treatment, which can result in rediffusion of the hydrogen from the metal and partially restore its ductility, should be at as high a temperature as the metallurgical condition of the component will permit without significant loss of other desirable properties (e.g. hardness or appearance). The time required to remove hydrogen from steel to avoid embrittlement depends on various factors including the strength of the steel. Longer treatment periods and higher temperatures are needed as the strength of steel increases. The use of inhibitors in the pickling process can also minimize the effects of hydrogen embrittlement, although some inhibitors, especially those containing certain organic sulfur compounds, actually promote hydrogen absorption. C2 APPLICATION C2.1 Preplating heat treatment Residual stress is not always undesirable, e.g. in pretensioned springs and case-hatdened surfaces, but, in most other cases, before applying. the chemical metal-finishing operation it is desirable to eliminate by heat treatment as much as possible of the residual stress resulting from mechanical operations such as grinding, polishing, cold working and also quench-hardening. Where parts have been tempered after hardening it is still considered necessary to stress-relieve after grinding and polishing because such processes can cause stress in the surface layers of the metal lating heat treatment Hydrogen generated from pickling and cleaning operations occurs to the greatest extent with cathodic treatment but may be minimized by anodic treatment. It can be assumed that some hydrogen is liberated at the work (cathode) during electroplating but in many cases the metal coating which has been deposited becomes a barrier to the diffusion of hydrogen into and out of steel. Cadmium, copper, nickel, nickel-chromium, tin, tin-nickel and zine coatings have similar barrier effects on the diffusion of hydrogen from the steel. Hard chromium plating from standard sulfuric chromic solutions is porous and heat treatment more readily removes hydrogen embrittlement (see AS 2453 for recommended heat treatment for hard chromium plating used in engineering applications). copyicHT‘Accessed by WOODSIDE ENERGY LTD on 19 Oct 2001 AS 162751994 1 Hydrogen absorption may also be influenced by other factors such as the presence of certain impurities or additives in the processing solutions (c.g. arsenic, phosphorus, and reduced sulfur compounds), the use of certain types of inhibitors and brighteners, and the nature of the deposits and conditions of plating, with the result that in some cases experimentation with the procedure may be necessary. C3 HEAT TREATMENT PROCEDURE €3.1 Before electroplating Items of highly work-hardened steel or steel having a tensile strength of 1000 MPa or higher, and which have been subject to grinding or severe mechanical working after tempering, should be heat treated in accordance with Table CL TABLE CL TYPICAL PREPLATING HEAT TREATMENT OF STEEL FOR STRESS RELIEF Metallurgical history Heat treatment Unknown prior to hardening heat testment 130°C to 210°C for 60 min to 30 min, respectively Highly cold-worked steels, nitrided steels and} 175°C 40 208°C for 30 steels of tensile strength grester than 1000 MPa (Rockwell hardaess: C30) Known hardening and tempering treatment Prom 130°C up to known tempering temperature for 60 min C3.2 After electroplating Items of highly work-hardened steel, surface-hardened steel or steel having a tensile strength of 1000 MPa or more require heat-treatment within four hours of plating in order to reduce the risk of the base metal being embrittled by hydrogen. Suitable heat treatment times and temperatures are given in Table C2. Where items have been zine or cadmium electroplated, heat treatment is carried out before the application of a chromate conversion coating, NOTE: Corrosion protection afforded by chromate conversion coatings is destroyed at the temperatures involved in the relief of hydrogen embrittlement. COPYRIGHT‘Accessed by WOODSIDE ENERGY LTD on 19 Get 2001 » AS 1627.5 —1998 TABLE C2 TYPICAL HEAT TREATMENTS FOR STEEL FOR STRESS RELIEF AND RELIEF OF HYDROGEN EMBRITTLEMENT AFTER THE APPLICATION OF ELECTROPLATED DEPOSITS OF CADMIUM, COPPER, NICKEL, NICKEL-CHROMIUM, TIN, TIN-NICKEL AND ZINC ‘Metallurgical history Heat treatment Highly cold-worked steels, nitrided steels and steels of 1000 to 1400 MPa tensile strength (approx. equivalent to Rockwell hardness C30 to C44) 200 #10°C for 4h min, Surface-hardened steels (not nitrided) where hardness is greater than Rockwell C55 or equivalent 135 E10°C for 4h min, Surface-hardened. steels where hardness is Tess than Rockwell C35 or equivalent 200 10°C for 4h min |All spring steel components, 130 #10°C for periods of up to 24 h depending upon aavice from the purchaser Highly cold-worked or hardened and tempered steel of tensile strength greater than 1400 MPa but less then 1750 MP3 200 £10°C for 18 b min Highly cold-worked or hardened and tempered steel of tensile strength greater chan 1750 MPa 200 *10°C for 24 h min.F See AS 2493 for the recommended heat treatment for items plated with had or porous chromium for engineering. applications. + Some coated steels may require « considerably greater time 10 achieve hydrogen embritlement relief. COPYRIGHT1002190 61 0.11 ADHINS 3O!SGOOM fa pessecoy