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THE ELECTROLYTIC PRODUCTION of PEROXYDISULFURIC ACID It USING PERIODICALLY REVERSED DIRECT CURRENT and ALTERNATING CURRENT SUPERIMPOSED on DIRECT CURRENT

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THE ELECTROLYTIC PRODUCTION OF PEROXYDISULFURIC ACID It USING PERIODICALLY REVERSED DIRECT CURRENT AND ALTERNATING CURRENT SUPERIMPOSED ON DIRECT CURRENT by Sin-Chou Fan Thesis submitted to the Graduate Faculty of the Virginia Polytechnic Institute in candidacy for the degree of MASTER OF SCIENCE in CHEMICAL ENGINEERING APPROVED: APPROVED: ~rector of Graduate Studies Head of Department ~ean of'"Engineering Major· Professor v July, 1956 Blacksburg, Virginia -ii- TABLE OF CONTENTS Page I. INTRODUCTION • • • . • • • • . • • • 1 II. LITERATURE REVIEW . 3 Properties and Uses of Peroxydisulfuric Acid . 3 Methods of Preparing Peroxydisulfuric Acid • . 5 Chemical Methods of Preparing Peroxy- disulfuric Acid . 5 Electrolytic Methods of Preparing Peroxy- disulfuri c Acid • • • • • • • 6 Electrolysis with Periodically- Reversed Direct Current • • • • . 11 Definitions • • • • • • 11 Periodic Reverse Wave Forms • • 13 Use of Complex Wave Forms . 16 Periodic Reverse Electro- chemical Reaction • • • . 16 Limitations of Periodic Reverse Electrolysis • . 18 Current Reversal Equipment • 19 Electrolysis with Alteniating Current Superimposed on Direct Current • • • • • • • . 20 Electric Double Layer . 20 -iii- Page Polarizable Electrode • • • • • 21 Types of Superimposed Alternating Current • • • • • 23 Depolarization by Alter- nat~ng Current • • • • • • • • 26 Experimental Work on Alternating Current Depolarization • • • . 34 Electrolysis of Sulfuric Acid with Alternating Current Superimposed on Direct Current • • • • • • 40 Applications • • • • • • 43 Electrolytic Production of Lead Chromate Using Alternating Current Superimposed on Direct Current • • • • • • 44 Other Applications • • • • . 46 Advantages of Alternating Current Superimposed on Direct Current • • • • • . 47 Comparison of Superimposed Alternating Current Plating with Periodic Reverse Current Plating . Electric Circuits for Superimposing Alternating Current • • • • • • • • . 50 III. EXPERIMENTAL • • • • . • • • . 57 Purpose of Investigation • • • • • • 57 -iv- Page Plan of Investigation • • . 57 Literature Search . 57 General Procedure . 58 Evaluation of Results . 59 Materials • • • • . 60 Apparatus • • . • • • • • . 62 Method of Procedure • • • • . 67 Operating Procedure for Direct Current Electrolyses • • • • • . 67 Operating Procedure for Periodically-Reversed Direct Current Tests • . 71 Operating Procedure for Electrolyses Performed with Alternating Current Superimposed on Direct Current • • • • • • • • • • • 73 Relationship Between Root- Mean-Square and Peak Values of High Frequency Alternating Current ••• . 76 Operating Procedure for Measuring Anode Potential- Current in Sulfuric Acid • . 76 Operating Procedure for Measuring the Anode Potential-Current in Sulfuric Acid with Super- imposed Alternating Current • • • • • • • • • • • 78 Analytical Procedure • . 78 -v- Page Data and Results . 80 Calibration Data for the Periodic Reverser • • . 80 Periodic Reverser Calibra- tion Curves • • • • • • • • • 80 Operating Conditions, Data and Results for the Elec- trolytic Production of Peroxydisulfuric Acid Using Direct Current • • • . 80 Operating Conditions, Data and Results for the Elec- trolytic Production of Peroxydisulfuric Acid Using Periodically Reversed, Direct Current • • • • • • • • 80 Operating Conditions, Data and Results for Electro- lytic Production of Peroxy- disulfuric Acid Using Alternating Current, 60 Cycles per Second, Super- imposed on Direct Current • • 84 Operating Conditions, Data and Results for the Elec- trolytic Production of Peroxydisulfuric Acid Using Alternating Current, 240 and 500 Cycles per Second, Superimposed on Direct Current • • • • • • • • • • • 84 Data from the Measurements of Current-Anode Potential Curve in Sulfuric Acid with Stirring • • • • • • • • • • • 84 -vi- Page Data from the Measurements of Current-Anode Poten- tial Curve in Sulfuric Acid without Stirring • • • • 89 Data from the Measurements of Current-Anode Poten- tial Curve in Sulfuric Acid by Using 60 Cycles per Second, Superimposed Alternating Current • • • • • 89 Sample Calculations ••• . 92 Volume of Anolyte . 92 Anode Current Density • • • 94 Peroxydisulfuric Acid Produced • • • • . 95 Actual Current • • • • . 96 Current Efficiency • . 97 Direct to Reverse Current Ratio from Coulometers • • • • 98 Ratio of Peak Alternating Current to Direct Current . 100 IV. DISCUSSION • . 101 General Discussion . 101 Previous Work . 101 Selection of Anolyte Concentration • • . • • 102 Influence of Temperature on the Formation of Peroxy- disulfuric Acid • • • • • 103 -vii- Page Treatment of Platinum Anode • • • • • • . 104 Influence of Current Density • • • • • • • • • • • 105 Formation and Decomposition of Peroxydisulfuric Acid • • • 106 Decomposition Potential of Sulfuric Acid of Specific Gravity 1.4 •• . 107 Discussion of Results from Direct Current Electrolyses • • 113 Hydrogen and Oxygen Bubbles • • 113 Effect of Current Density • • • 113 Relationship Between the Time of Electrolysis and Current Efficiency . 118 Discussion of Results for Periodically-Reversed, Direct Current Electrolysis • • • • 121 Production of Peroxydisul- furic Acid Using Period- ically-Reversed, Direct Current • • • • • • • • • • • 121 Depolarization Action of Periodically-Reversed, Direct Current • • • • . • • 123 Ammeter Fluctuations During Current Reversal • • • ~ • • • 125 Time and Current Ratio • . 128 Comparison of Current Efficiencies • • • • • • • • • 129 -viii- Page Discussion of Results from Alternating Current Super- imposed on Direct Current Electrolyses • • • • • • • • • • • 131 Formation of Peroxydisul- fµric Acid with 60-Cycle, Alternating Current Super- imposed on Direct Current • • 131 Formation of Peroxydisul- furic Acid with 500-Cycle, Superimposed Alternating Current • • • • • • • • • • • 135 Formation of Pero:x:ydisul- furic Acid with 240-Cycle Alternating Current Super- imposed on Direct Current • • 136 Summary of Effect of Frequency • • • • • • • • • • 136 Behavior of Platinum Electrode • • • • • . Current Efficiency • • • • • . Comparison of Current Efficiencies • • • • . • • • 139 Recommendations • • • • • • . 142 Limitations • • • • • • . 145 v. CONCLUSIONS - • • • • • • • • • • . 148 VI. SUMMARY • • • • • • • • • • • • • • • • • 151 VII. BIBLIOGRAPHY • • • . • • • • • . 155 VIII. ACKNOWIEDGMENTS . 162 IX. VITA • • • • • • . • • 163 -ix- LIST OF TABLES Page TABLE I. Calibration Data for Plater's Research Corporation ' Periodic Reverser . • . • • 81 TABLE II. Operating Conditions, Data and Results Obtained from the Electrolytic Production of Peroxydisulfuric Acid . • • . • • 83 TABLE III. Operating Conditions, Data and Results Obtained from the Electrolytic Production of Peroxydisulfuric Acid Using Periodically-Reversed, Direct Current . • • • • . • 85 TABLE IV. Operating Conditions, Data and Results Obtained from the Electrolytic Production of Peroxydisulfuric Acid Using Alternating Current, 60 Cycles, Superimposed on Direct Current . • . • • • . • 86 TABLE v. Operating Conditions, Data and Results Obtained from the Electrolytic Production of Peroxydisulfuric Acid Using High Frequency of Alternating Current Superimposed on Direct Current . • • • • . • . 87 TABLE VI. Data from the Measurements of Current-Anode Potential Curve in Sulfuric Acid with Stirring • • . • • • • . • • 88 TABLE VII. Data from the Measurements of Current-Anode Potential Curve in Sulfuric Acid without Stirring • • • • • • . • 90 -x- Page TABLE VIII. Data from the Measurements of Current-Anode Potential Curve in Sulfuric Acid Using Superimposed alternating Current • • • • • • • • • • • • • 91 -xi- LIST OF FIGURES Page Figure 1. Time-Current Curves for Various Wave Forms . • • • . • 17 Figure 2. Representation of the Poten- tial-Distance Relation for the Electrode-Solution Interface . • • • . • • • • . • 22 Figure 3. Time-Current Relations for Alternating Current Superimposed on Direct Current • • . • . • • • • . 24 Figure 4. Experimental Hook-Up Used to Study the Effect of Super- imposed Alternating Current on Direct Current on the Electrodeposition of Aluminum . • • . • . • • • • . • . 52 Figure 5. Experimental Hook-Up Used to Study the Effect of Super- imposed Alternating Current on Direct Current on the Anodic Behavior of A-A Type Nickel . • . • . • 53 Figure 6. Experimental Hook-Up Used to Study the Effect of Super- imposed Alternating Current on Direct Current on the Anodic Behavior of Nickel . • • 55 Figure 7. Experimental Hook-Up Used to Study the Effect of Super- imposed Alternating Current on Direct Current on the Electrodeposition of Copper- Lead Alloys from Fluoborate Solutions • • • . • • . • 56 -xii- Page Figure 8. Wiring Diagram of Equipment Used to Study the Electro- lytic Production of Peroxy- disulfuric Acid Using Direct Current • • • • • • • . 69 Figure 9. Wiring Diagram of Equipment Used to Study the Electro- lytic Production of Peroxy- disulfuric Acid Using Periodically Reversed Direct Current • • • • • • . 72 Figure 10. Experimental Circuit Used to Study the Effect of Super- imposed Alternating Current on the Production of Peroxy- disulfuri c Acid • • • • • • • • • 74 Figure 11. Experimental Circuit Used for Measuring Current-Anode Potential Curve • • • • • • . 77 Figure 12. Graph Showing the Relationship Between the Ratio of Direct to Reverse Time and the Dial Settings for the Periodic Reverser • • • • • • • • • • . 82 Figure 13. Relationship Between Current and Anode Potential in Sulfuric Acid with Stirring . 108 Figure 14. Relationship Between Current and Anode Potential in Sulfuric Acid without
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    GUIDELINES FOR THE PRESERVATION OF RAW MILK BY USE OF THE LACTOPEROXIDASE SYSTEM CAC/GL 13-1991 INTRODUCTION Milk is an easily perishable raw material. Contaminating bacteria may multiply rapidly and render it unsuitable for processing and/or unfit for human consumption. Bacterial growth can be retarded by refrigeration, thereby slowing down the rate of deterioration. Under certain conditions refrigeration may not be feasible due to economical and/ or technical reasons. Difficulties in applying refrigeration are specially a problem for certain areas in countries setting up or expanding their milk production. In these situations, it would be beneficial to have access to a method, other than refrigeration, for retarding bacterial growth in raw milk during collection and transportation to the dairy processing plant. In 1967 the FAO/WHO Expert Panel on Milk Quality concluded that the use of hydrogen peroxide might be an acceptable alternative in the early stages of development of an organized dairy industry, provided that certain conditions were complied with. However, this method has not achieved any general acceptance as it has several drawbacks, most important of which is the difficulty of controlling its use: it may be misused to disguise milk of basic hygienic quality produced under poor hygienic conditions. The toxicological aspects of the use of relatively high concentrations of hydrogen peroxide in milk have also been questioned. A chemical method for preserving milk would still be of great advantage in certain situations. The search for such a method has therefore continued. Interest has recently been focused on the indigenous antibacterial systems in milk to determine if these could be applied practically to preserve raw milk.
  • Chemical Names and CAS Numbers Final

    Chemical Names and CAS Numbers Final

    Chemical Abstract Chemical Formula Chemical Name Service (CAS) Number C3H8O 1‐propanol C4H7BrO2 2‐bromobutyric acid 80‐58‐0 GeH3COOH 2‐germaacetic acid C4H10 2‐methylpropane 75‐28‐5 C3H8O 2‐propanol 67‐63‐0 C6H10O3 4‐acetylbutyric acid 448671 C4H7BrO2 4‐bromobutyric acid 2623‐87‐2 CH3CHO acetaldehyde CH3CONH2 acetamide C8H9NO2 acetaminophen 103‐90‐2 − C2H3O2 acetate ion − CH3COO acetate ion C2H4O2 acetic acid 64‐19‐7 CH3COOH acetic acid (CH3)2CO acetone CH3COCl acetyl chloride C2H2 acetylene 74‐86‐2 HCCH acetylene C9H8O4 acetylsalicylic acid 50‐78‐2 H2C(CH)CN acrylonitrile C3H7NO2 Ala C3H7NO2 alanine 56‐41‐7 NaAlSi3O3 albite AlSb aluminium antimonide 25152‐52‐7 AlAs aluminium arsenide 22831‐42‐1 AlBO2 aluminium borate 61279‐70‐7 AlBO aluminium boron oxide 12041‐48‐4 AlBr3 aluminium bromide 7727‐15‐3 AlBr3•6H2O aluminium bromide hexahydrate 2149397 AlCl4Cs aluminium caesium tetrachloride 17992‐03‐9 AlCl3 aluminium chloride (anhydrous) 7446‐70‐0 AlCl3•6H2O aluminium chloride hexahydrate 7784‐13‐6 AlClO aluminium chloride oxide 13596‐11‐7 AlB2 aluminium diboride 12041‐50‐8 AlF2 aluminium difluoride 13569‐23‐8 AlF2O aluminium difluoride oxide 38344‐66‐0 AlB12 aluminium dodecaboride 12041‐54‐2 Al2F6 aluminium fluoride 17949‐86‐9 AlF3 aluminium fluoride 7784‐18‐1 Al(CHO2)3 aluminium formate 7360‐53‐4 1 of 75 Chemical Abstract Chemical Formula Chemical Name Service (CAS) Number Al(OH)3 aluminium hydroxide 21645‐51‐2 Al2I6 aluminium iodide 18898‐35‐6 AlI3 aluminium iodide 7784‐23‐8 AlBr aluminium monobromide 22359‐97‐3 AlCl aluminium monochloride
  • SAFETY DATA SHEET Sodium Persulfate

    SAFETY DATA SHEET Sodium Persulfate

    SAFETY DATA SHEET Sodium Persulfate SDS # : 7775-27-1 Revision date: 2021-02-17 Format: NA Version 1.06 1. PRODUCT AND COMPANY IDENTIFICATION Product Identifier Product Name Sodium Persulfate CAS-No 7775-27-1 Synonyms Sodium Peroxydisulfate; Disodium Peroxydisulfate; Peroxydisulfuric acid, disodium salt; Peroxydisulfuric acid, sodium salt. Recommended use of the chemical and restrictions on use Recommended Use: Polymerization initiator; Etchant and cleaner for printed circuit boards; Hair bleaching formulations; Secondary oil recovery; Oxidizing agent for a variety of organic reactions. Restrictions on Use No uses to be advised against were identified. Manufacturer/Supplier PeroxyChem LLC 2005 Market Street Suite 3200 Philadelphia, PA 19103 Phone: +1 267/ 422-2400 (General Information) E-Mail: [email protected] Emergency telephone numbers For leak, fire, spill or accident emergencies, call: 1 800 / 424 9300 (CHEMTREC - U.S.A.) 1 703 / 527 3887 (CHEMTREC - Collect - All Other Countries) +1 303/ 389-1409 (Medical - U.S. - Call Collect) Page 1 / 10 Sodium Persulfate SDS # : 7775-27-1 Revision date: 2021-02-17 Version 1.06 2. HAZARDS IDENTIFICATION Classification OSHA Regulatory Status This material is considered hazardous by the OSHA Hazard Communication Standard (29 CFR 1910.1200) Acute toxicity - Oral Category 4 Skin corrosion/irritation Category 2 Serious eye damage/eye irritation Category 2B Respiratory sensitization Category 1 Skin sensitization Category 1 Specific target organ toxicity (single exposure) Category 3 Oxidizing Solids
  • 2 1 0 Material Safety Data Sheet

    2 1 0 Material Safety Data Sheet

    He a lt h 1 2 Fire 2 1 0 Re a c t iv it y 0 Pe rs o n a l Pro t e c t io n H Material Safety Data Sheet Methylene Blue Solution, Loeffler MSDS Section 1: Chemical Product and Company Identification Product Name: Methylene Blue Solution, Loeffler Contact Information: Catalog Codes: SLM3328 Sciencelab.com, Inc. 14025 Smith Rd. CAS#: Mixture. Houston, Texas 77396 RTECS: Not applicable. US Sales: 1-800-901-7247 International Sales: 1-281-441-4400 TSCA: TSCA 8(b) inventory: Potassium hydroxide; Ethyl alcohol 200 Proof; Water Order Online: ScienceLab.com CI#: Not applicable. CHEMTREC (24HR Emergency Telephone), call: 1-800-424-9300 Synonym: Methylene Blue-Loeffler's Alkaline International CHEMTREC, call: 1-703-527-3887 Chemical Name: Not applicable. For non-emergency assistance, call: 1-281-441-4400 Chemical Formula: Not applicable. Section 2: Composition and Information on Ingredients Composition: Name CAS # % by Weight Potassium hydroxide 1310-58-3 <1 Ethyl alcohol 200 Proof 64-17-5 25-30 Water 7732-18-5 70-75 Methylene Blue CI52015 7220-79-3 <1 Toxicological Data on Ingredients: Ethyl alcohol 200 Proof: ORAL (LD50): Acute: 7060 mg/kg [Rat.]. 3450 mg/kg [Mouse]. VAPOR (LC50): Acute: 20000 ppm 8 hours [Rat]. 39000 mg/m 4 hours [Mouse]. Section 3: Hazards Identification Potential Acute Health Effects: Hazardous in case of skin contact (irritant, permeator), of eye contact (irritant), of ingestion. Potential Chronic Health Effects: CARCINOGENIC EFFECTS: Classified PROVEN by State of California Proposition 65 [Ethyl alcohol 200 Proof]. Classified A4 (Not classifiable for human or animal.) by ACGIH [Ethyl alcohol 200 Proof].