degree of fire protection available are the prime factors determining rates. Structural design is secondary. Boiler and machine underwriters, who often insure process equipment against rup ture, consider each tank or vessel in dividually for coverage. While they are prone to check closely the design calculations for a noncode vessel, standard rates apply if the design of the vessel is approved by the under writers. Appendix R will supplement Stand ard 620 by recommending materials of construction for several ranges of design metal temperatures from - 6 0 ° F. to 40° F. It details impact test requirements for primary tank components, describes additional welding rules, and discusses test pro cedures beyond those for nonrefrigerated tanks. It covers both single-wall and double-wall designs. AS Μ Ε Code. Though the new por tion being developed for the ASME code has been tagged Section VIII Di vision 2, it hasn't been decided whether it will in fact be part of Sec tion VIII or a new code section in it self. The special committee, which has been working on this addition for about two years, was created in 1955 to review the entire code. Its first task—by popular demand—was to in corporate the most advanced design concepts in current use into a stand ard for vessels in nuclear service. This was accomplished in 1962 with the issue of Code Section III. The special committee is now at tempting to extend this thinking to large industrial vessels. One member of the code committee characterizes the work as a completely new ap proach to pressure vessel design. No extensive rewriting of present Section VIII is involved. The new provisions won't cover production line vessels such as air receiver tanks and similar vessels. The committee may take a look at extending Section VIII coverage be yond 3000 p.s.i.g. design pressure—its present limit. This has been consid ered and rejected several times in re cent years, however, since so few in dustrial vessels are built for such pressure. There is also some reluc tance to freeze specifications while ultrahigh-pressure technology is in a pe riod of rapid growth. As one commit tee member puts it, it is important to gain some experience with the new materials and designs now available before ASME says "thou shalt."
New Chemicals Pattern for Kraft Pulpers Could cut cost of kraft pulping and bleaching by as much as a quarter to a third No need to buy chlorine, caustic soda, or salt cake. This is the prospect held out to kraft pulpers—and to sup pliers of the chemicals—by a new chemical supply system for pulping and bleaching. Only sodium chlo rate, sodium chloride, and sulfuric acid, in addition to the usual lime, are required. The system, which its developers believe could cut bleaching costs by as much as a quarter to a third, is now in mill trials at the Crofton, B.C., mill of British Columbia Forest Products. If it proves out, it could be a shot in the arm for the so-called R2 process developed several years ago by Dr. W. Howard Rapson, professor of chemical engineering at the Univer sity of Toronto, along with Electric Reduction Co. of Canada (ERCO) and Hooker Chemical. Originally developed to produce chlorine dioxide for bleaching, the R2 process involves reactions of sodium chlorate, sodium chloride, and sulfuric acid. Besides chlorine dioxide and chlorine, however, sodium sulfate is also produced. Success had hinged on a method for crystallizing sodium sulfate from solution as Glauber's salt (sodium sulfate decahydrate) and evaporating and recycling sulfuric acid. It's this R2 process that's now the basis for the new chemical supply con cept. The concept was described by Dr. Rapson at the 50th Annual Meet ing of the Technical Association of the Pulp and Paper Industry, in New York. Even as he was speaking, ERCO engineers were starting up a new pilot plant on a revised R2 proc ess—a simpler one, with lower capital cost. The revised process is designed to produce anhydrous sodium sulfate and a more concentrated chlorine. Integrates. The new concept inte grates and changes somewhat the chemical flow patterns in pulping and bleaching. In a typical kraft pulp plant, pulp is digested with white liq uor, the fresh cooking liquor made up primarily of sodium sulfide and so dium hydroxide. After cooking, spent (black) liquor washed from the pulp goes to chemical recovery.
Pulp to be bleached then goes to a chlorination stage in the bleaching op eration. Chlorinated alkali lignin, however, is almost insoluble in acid solution; so chlorination is followed by caustic extraction with sodium hy droxide. The pulp is then further bleached with sodium hypochlorite or chlorine dioxide. Another caustic ex traction follows. Back in the pulping operation, black liquor that has entered the chemical recovery system is evapo rated (and tall oil skimmed off) and sent to a combustion furnace. There it burns to a molten mixture of pri marily sodium carbonate and sodium sulfide. The melt discharges to a quench tank to form green liquor, which is then causticized with lime to convert the sodium carbonate to so dium hydroxide. The calcium carbon ate that forms in this step is filtered and burned to calcium oxide, availa ble again for causticizing. The re maining solution, white liquor, is ready for feeding to the digesters. To make up sodium sulfide losses in the pulping process, salt cake (crude sodium sulfate) is added to the solu tion entering the furnace. It is re duced in a furnace to sodium sulfide. Thus a kraft mill generally buys salt cake for makeup, chlorine for bleaching, and sodium hydroxide for caustic extraction and for making so dium hypochlorite. It also buys so dium chlorate, sulfuric acid, and ei ther sulfur dioxide, methanol, or sodium chloride for reducing sodium chlorate to chlorine dioxide. Added to these is calcium carbonate or lime for recausticizing. All told, Dr. Rapson says, chemicals used to make bleached kraft pulp range on an aver age from $13 to $17 per ton of pulp. Change Supply. Two factors ac count for the R2 process being able to change this supply picture. First, the process makes both chlorine and chlorine dioxide, and it can be ad justed to give these in whatever pro portion is needed. Second, labora tory experiments and mill operation have shown that it's perfectly feasible to use white liquor instead of sodium hydroxide for caustic extraction. MAR.
3, 1965
C&EN
69
Two reactions take place in the R2 generator, Dr. Rapson explains. In the first, one mole each of sodium chlorate, sodium chloride, and sul furic acid react to give one mole each of chlorine dioxide, sodium sulfate, and water, along with a half mole of chlorine. In the other, one mole of the chlorate, five of the chloride, and three of sulfuric acid give three moles each of chlorine, sodium sulfate, and water. Any ratio of one reaction to the other can be produced, Dr. Rapson says, by varying the ratio of sodium chlorate to sodium chloride in the feed and by maintaining acidity by adding sulfuric acid when necessary. This means that the chlorine-to-chlo rine dioxide ratio can be varied over a wide range, and, further, by varying this ratio, more or less salt cake can be produced. In this way, enough salt cake can be made to meet white liquor require ments for both pulping and caustic extraction. However, Dr. Rapson points out, the cost of chemicals to the mill will be closer to a minimum, the closer the generator can be operated to the first reaction and still meet bleaching and salt cake needs. A limited amount of water dissolves preferentially about 40% of the chlo rine dioxide in the chlorine/chlorine
dioxide mixture from the process. This is used for the latter stages of bleaching. The remaining chlorine dioxide and most of the chlorine are dissolved in a larger amount of water for use in the chlorination stage. As an additional way of cutting costs, a sizable amount of sodium salts can be recovered from the first caustic extraction stage. Putting this back into the system would reduce the sodium sulfate production needs from the R2 process and thus allow the process to be operated closer to the preferred first reaction. The best place to put the caustic extraction filtrate back into the system is as part of the water supplied for making green liquor. This, however, could pose a poten tial problem and is one of the points being studied in the mill tests. The problem arises because some of the chlorine from chlorination shows up in the caustic extraction as chlorides. As extraction filtrate recycles, chlo rides will build up in the system. Dr. Rapson says that opinions vary as to whether there is a corrosion or explosion hazard caused by a high chloride content in the system. He points out, though, that high chloride concentrations are found normally in white liquor in coastal mills using logs floated in sea water.
White Liquor Replaces Sodium Hydroxide for Caustic Extraction Chlorine/Chlorine dioxide Water
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MAR. 8, 1965
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Treated Salt Removes Snow While Reducing Auto Corrosion If snow on some highways in the up per Midwest has an unusual char treuse tinge next winter it will not be due to the whim of a highway engi neer with a keen sense of the aes thetic. It will be due to Carguard, the new treated salt made by Cargill, Inc., the Minnesota grain handler, for removing ice and snow from high ways. Cargill has been testing the new salt for three years and claims that it cuts the rusting of autos by as much as 84% compared to regular salt. The color is incidental—caused by ad ditives in the product. Salt currently used on highways is not generally treated by the compa nies that produce it to cut corrosion. Salt companies have been working on treated salts for some years, but have shied away from putting them on the market, mainly because of cost. Also, the effectiveness of these treated salts in reducing auto rusting has not been fully established under field condi tions. Cargill now thinks that it has over come these problems by developing a salt with good anticorrosion proper ties at a price that can still attract customers. Delivered price of un treated highway salt is about $8.00 to $15 per ton, depending on transpor tation costs. Carguard will be about $4.00 per ton more. Additives. The new product con sists of rock salt plus five additives. Four of these are to inhibit rust. The fifth, sodium ferrocyanide, is an anticaking agent commonly used in high way salts. These additives total less than 1 % by weight of the product. Carguard inhibits rust by hamper ing the electrochemical reaction that is the key to the corrosion of iron. In the presence of moisture, cathodic and anodic areas are set up on the surface of the metal. These trigger corrosion. The additives in Carguard protect these areas separately—the cathodic areas with a film, the anodic areas by a catalytic reaction. The metallic salt of a long-chain or ganic compound protects the cathodic areas. It forms a film when the posi tive (metallic) ends of the molecules attach themselves to these negatively charged areas. As a result the longchain ends stand out like the fibers on a carpet. The film slows corrosion of these areas by electrically insulating
GAS CHROMATOGRAPHY Whatever you analyze... WCLID* Series 1600 gives you specificity, adaptability and a week-long seminar on laboratory applications
In the clinical laboratory steroids · f a t t y acids · blood alcohols barbiturates · alkaloids
In the industrial laboratory Applications a s diverse a s your analytical p r o b l e m s ! (A few of the many substances which have been analyzed gas chromatographically : alcoholic beverages · drugs · pesticides · essen tial oils · water · atmospheric gases * detergents)
POWER SUPPLY TEMPERATURE CONTROLLER
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BETA OR ELECTRON CAPTURE DETECTOR
TEMPERATURE CONTROLLER
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SINGLE OR DUAL HYDROGEN FUME DETECTORS
ELECTROMETER AMPLIFIER
LONG COLUMN OVEN
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WCLID MODEL #1662-E, $2,250.00, EXCLUSIVE OF STRIP CHART RECORDER
Specify a single clinical application—and the 1600 series has a mod ular system for runnins: your determinations. No need to order components you'll never need or use. If your use of gras chromatog raphy expands, your system expands—with additional modules.
Purchasers of WCLID gas chromatography systems (series 1600) are eligible for a weeklong free seminar on practical applications. (Biomedical and Industrial seminars to be held on alternate weeks.) Classes may be at tended by any members of your laboratory staff who will be using the chromatography equipment. Interested? Return the coupon. The GENERAL DIAGNOSTICS/WARNER CHILCOTT LABORATORIES I N S T R U MENTS DIVISION, Department of Techni cal Education conducts shorter seminars on thin-layer, column and paper chromatogra phy ; on electrophoresis, enzymology, coagu lation and quality control.
COILED COLUMN OVEN
FLOW CONTROL
Adapt the 1600 series to almost any industrial application—simply by changing the modules. Select the type of detector you need: hydrogen flame, thermal conductivity, beta-ionization. Select the sampling: valve, input splitter, flow meter. The 1600 series is as adaptable as your needs·
| I'd like to know more about the WCLID Gas Chromatography system and the seminars on laboratory applications.
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*Warner-Chilcott Laboratories Instruments Div. Morris Plains, N.J.
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CORROSION PITS. Young Joo Lee, Cargill chemist, measures depth of corrosion pits in auto body metal exposed to salt. Cargill's Carguard contains a rust inhibitor to reduce these pits caused by deicing salt
them. It also keeps oxygen from them. However, the most severe corrosion takes place at the anodic areas. Here iron is first converted to ferrous hydroxide. When chlorides are present, this hydroxide forms ferrous and ferric chlorides. Because these iron chlorides are very soluble, they are easily washed away. This leaves sites for continued corrosion. Carguard inhibits this anodic corrosion by catalyzing the conversion of the ferrous hydroxide to gamma ferric oxide. This iron oxide forms a dense film that adheres to the metal surface, preventing further rusting. Cargill will not name this catalytic additive nor will it talk about the third and fourth anticorrosion additives. But Dr. Russell Eversole and Young Joo Lee, the chemists who developed Carguard, say that these two are minor components that aid the function of the film forming and catalytic additives. Tests. Cargill started testing treated salts in the winter of 1962-63 at about the same time as the company became a basic salt producer with its Belle Isle, La., rock salt mine. 72
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8,
1965
The first year's tests were encouraging but very limited. A more ambitious testing program for 1963-64 was frustrated by a lack of snow. But this winter Cargill feels that it has been successful in showing the performance of the new salt. A field test is being run at Davenport, Iowa, where three areas in a city park have been set aside. One of these areas is treated with Carguard, one with regular salt, and the other is not treated. Test autos are driven over these areas for about 60 min. per day. Steel test panels are attached under the fenders of these autos. Every two weeks a few are removed, examined, cleaned, and weighed. Some of the panels are flat, others have a V-notch in them. After 10 weeks, the flat panels exposed to Carguard have lost only 16% as much weight as have the panels exposed to regular salt, according to Cargill. Dr. Eversole expresses this result as 84% protection for the Carguard panel. The corresponding notched panels show 57% protection. And the Carguard panels have lost less weight than have the panels exposed to unsalted snow. These tests
will run for a total of 12 weeks. However, Dr. Eversole points out that previous tests indicate that the last two weeks will not change these 10week results significantly. These results are of the same order as those obtained by a research foundation, according to Cargill. In those tests metal panels were exposed to Carguard, regular salt, or water under laboratory conditions that simulated 12 weeks of commuter driving during a rigorous snow season. The flat panels exposed to Carguard showed 78% protection and the notched panels 57% protection compared to regular salt. Furthermore, Carguard panels showed 2 1 % protection compared with those panels exposed to moisture only. Cargill is encouraged by these results. It feels that this corrosion protection will attract highway engineers in spite of the premium cost. Cargill already has plans beyond Carguard. Evan Williams, sales official of the company's salt department, says that Cargill may offer the additives in Carguard as a package which can be blended into either salt or calcium chloride. Cargill also may license other companies to make a treated salt just like Carguard. C 34
Epoxy Cures in Thin Film At Low Temperatures An epoxy resin system that will cure in thin films at temperatures as low as 0° F. has been developed by Adhesive Engineering Co., of San Carlos, Calif. The system can be used to make a series of epoxy products that cure at normal temperatures with speeds not attainable before. Concressive Series 1200 is available in four formulations—two liquids and two pastes, with a flexible and rigid form for each. Epoxies of this group will cure within two to five hours in thin films compared to the usual cure time of five to seven days for conventional products with the same working life in a large mass. Most of the epoxy products developed from this line will cure in 30 hr. at 0° F . and from 30 min. to one hour at room temperature (60° to 80° F.). The effective pot life of these epoxies runs from 20 min. to one hour. However, one special epoxy formulation in the group will cure in about five minutes but has an effective pot life of only one to two minutes.
Adhesive Engineering says that the epoxies can be used in aerospace and construction industries. They can also be used in electrical equipment manufacture, light metal assembly, and laminating. Highway patching and bridge sealing at low tempera ture are also possible. C 35
New Preservative
dioxin
*
BRIEFS Chemical resistance properties of commercially available carbon and graphite can be upgraded by a process developed by General Electric Co.'s Metallurgical Products department at Detroit, Mich. The process consists of impregnating commercial carbons and graphites with pyrolytic graphite by vapor deposition. According to the company, the impregnation proc ess increases bulk density, thermal conductivity, and flexural, tensile, and compression strengths. At the same time, fluid permeability, bulk resistiv ity, and chemical reactivity are re duced, GE says.
(Brand of Dimethoxane)
Broad-Spectrum Antimicrobial Agent
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Eighteen new color charts are avail able from the National Bureau of Standards. They are for use in stud ies of trends in color use, in coordi nating colors in lines of merchandise, and for standardizing the colors of manufactured goods. The charts are designed for use with NBS Circular 553 which describes a method for designating colors and contains a dic tionary of color names. The charts may be ordered as Standard Material 2106 from the Office of Standard Ref erence Materials, National Bureau of Standards, Wash., D.C. ($3.00). Circular 553 is available from the Superintendent of Documents, U.S. Government Printing Office, Wash ington, D.C. ($2.00).
H30
0 GHCH.
Rarely Inactivated Low Toxicity
Dioxin effectively and safely controls the numerous spoilage microorgan isms found in water systems and emulsions. When added to severely con taminated systems, 9 9 % kill is usually achieved, regardless of pH or composition. Dioxin works in cutting oils, resin emulsions, water-based paints, cosmetics, inks, textile and paper emulsions,—even in the pres ence of nonionic surfactants. For more details please send us this coupon:
A process for recovering vanadium from mining wastes has been devel oped by research workers at Colorado School of Mines Research Founda tion. After oxidation of the vanadium by the addition of sodium chlorate, activated charcoal is used to adsorb the vanadium. Desorption by an al kaline reagent and precipitation of the highly pure vanadium with sulfuric acid follow. The study was sup ported by West Virginia Pulp and Paper Co/s Covington, Va., carbon plant.
CHCH3
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3 2 1 West 4 4 t h Street, New York, N.Y.
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MAR. 8, 196 5 C & E N
73
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PROGRESS REPORT
These items have all been mentioned editorially in C&EN in the past month. If you haven't already sent for information on them, just check the appropriate key numbers on the coupon on page 76, and C&EN's Readers' Information Service will forward your request to the manufacturer.
INSTRUMENT AND CONTROLS . . . Product
Company Capital Controls Co., Inc. Col mar, Pa. Corning Glass Works Corning, N.Y.
Gas chlorinator
Ε 60
pH meter
Ε 61
Integrator
Ε 62
Color comparator
Ε 63
Dielectric measurements (DM 01 Diplometer)
Ε 64
Kahl Scientific Corp. El Cajon, Calif.
Calorimeter (Model AC-1000) Chromatography assembly
Ε 65
Thermo-Physics Corp. Cambridge, Mass. Water Associates, Inc. Framingham, Mass.
Ε 66
Fischer and Porter Co. Warminster, Pa. Hach Chemical Co. Ames, Iowa
Features Automatic switch-over system for con tinuous treatment of process waters Control knob permits full-scale deflec tion of any 3-pH unit range with rela tive accuracy of 0.01 pH Will totalize, with respect to time, a linear or square root flow signal For colorimetric liquid analysis of vari ous metal ions including chlorine, iron, copper, and manganese For molecular structure confirmation, dielectric investigations, and quality control For determining specific heat and heat of reaction of materials For analyzing polymer molecular weights for both average number and average weight
EQUIPMENT AND LABWARE . . . Cryogenic piping
Ε 67
Boilers (Cyclopak) Hardness tester (Sonodur Model 100) Thermocouples (Con-O-Clad) Flotation mechanism (D-R) Pressure transmitters
Ε 68
Copper electrodes
Ε 69 Ε 70 Ε 71 Ε 72 Ε 73
Miniature valves
Ε 74
Mica gaskets
Ε 75
Plastic pipe
Ε 76
Hydraulic press (Model C-30) Support materials (Fiberfilm)
Ε 77 Ε 78
Ribbon mixer
Ε 79
Immersion heaters
Ε 80
Dehumidifier (Model A-220)
Ε 81
Plastic pumps
Ε 82
74
C&EN
MAR. 8, 196 5
Ι Air Reduction Co., Inc. New York, N.Y. Babcock & Wilcox Co. New York, N.Y. Branson Instruments, Inc. Stamford, Conn. Conax Corp. Buffalo, N.Y. Denver Equipment Co. Denver, Colo. Foxboro Co. Foxboro, Mass. Heli-Coil Corp. Danbury, Conn. Hills-McCanna Co. j Carpentersville, III. Industrial Mica Corp. Woodside, N.Y. Lamtex Industries Farmingdale, L.I-, N.Y. Limit Research Corp. Darien, Conn. Pallflex Products Corp. Putnam, Conn. Patterson Industries, Inc. East Liverpool, Ohio Sethco Mfg. Co. Freeport, N.Y. Universal Dynamics Corp. Alexandria, Va. Vanton Pump and Equi Corp. Hillside, N.J.
Semiflexible piping constructed of con voluted copper tubing Packaged units will generate up to 200,000 lb. per hour of steam Ultrasonic unit which does not require high-pressure contact or impact For use in hydrogen, nitrogen, inert, or high-vacuum atmospheres Impeller mechanism gives improved efficiency of flotation machines For use with low-pressure fractionating columns, evaporators, or degassing equipment Designed for electric discharge and elec trochemical machinery Available in a variety of body, bonnet, and diaphragm combinations (%-, Vt, and % - i n . size valves) For use in high-pressure, high-tempera ture boilers and chemical vessels Filament-wound, glass fiber-reinforced epoxy pipe and polyester tubing For pelletizing potassium bromide and similar press projects For electrophoresis analysis or chroma tography (available in rolls of i/ 2 -, 1-, and 12-in. widths) Dual-purpose mixer and disintegrator produces a uniform finished mix Acid-resistant units designed for lab oratory or pilot-plant tanks Removes up to 900 lb. of moisture per day with a rated airflow of 1500 cu. ft. per minute For automatic pumping of many cor rosive and/or viscous materials
NEW CHEMICALS Nylon injection
molding resins
are
offered by Spencer Chemical divi sion of Gulf Oil Corp. According to the Kansas City, Mo., company, the X-tal resins, because of their fast rate of setup from the melt, enable molders to achieve much shorter ma chine cycle time. C 30
Diiron nonacarbonyl and triiron dodecacarbonyl are available from Alfa Inorganics, of Beverly, Mass. The iron carbonyls are useful as in termediates in the synthesis of iron carbonyl derivatives. C31
Quartz Co., of Philadelphia, Pa. Quram 223 shows excellent binding ability in refractory materials and imparts water, weather, and heat re sistance to protective coatings, the company says. C 32
Thioglycolic acid is available from Halby Products Co., Inc., of Wil mington, Del. The acid is used in the manufacture of vinyl stabilizers and depilatories and as a reagent for metal analysis. C 33
Further information on keyed Equipment and Chemicals items is readily available . . .
Organic ammonium silicate, Quram 223, is available from Philadelphia
Use handy coupon on page 76
March 8, 1965
Readers' Information Service
Use this handy self-mailer to obtain further information or literature. Simply mark the items desired, fill out the information requested, clip the coupon, fold, staple, and mail.
Name: Company: Street: Zone-
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POLYFUNCTIONAL MERCAPTANS Carlisle's MERCAPTATE* Esters provide a n e w means of modi fying p o l y m e r i z a t i o n reactions. T h r e e m e m b e r s t y p i c a l of t h e series are pictured above. Other k n o w n uses include plasticizers, curing agents, and polymerization modifiers. Perhaps you have still another. PROPERTIES
YOUR FUNCTIONS (Maximum of 2, please.) Α Β C D Ε F
Π Π Π Π Π Π
Management Process Research & Development Product Research & Development Basic Research Plant Operations Engineering Design & Construction
GΠ ΗΠ Ι Π J Π ΚΠ
Analysis/Testing Marketing/Sales Purchasing Consulting Teaching—Student
The MERCAPTATE Esters are high-boiling, vis cous liquids. They have sharp, sulfur-like odors. They are insoluble in water and the alkanes, but are soluble to varying degrees in other organic solvents. Reactions of the MERCAPTATE Esters are typi cal of both the mercaptan and the ester.
AVAILABILITY CLIP COUPON—Fold along this line—fasten (staple, tape, glue) MAIL
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Κ ( ) Petroleum Réf., Asphalts, Lubricants L ( ) Rubber and Plastic Products M ( ) Independent Laboratories Ν ( ) Consultants 0 ( ) Primary Metal Industries Ρ ( ) Fabricated Metal Products Q ( ) Machinery and Equipment R ( ) Transportation Equipment S ( ) Instruments and Controls Τ ( ) Education
Six types of MERCAPTATE Esters are avail able immediately in development quantities. Detailed information on MERCAPTATE Esters is carried in Bulletin D-103. Write for a copy. Better still, if you would like to discuss your needs, call us at area code 513, 821-3660, and ask for Bob Witman or Paul Thompson. *T.M.,C.C.W.
CARLISLE
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