EQUIPMENT
New Mass Spectrometer in Production British firm makes first shipments of new instrument designed for high resolution studies of organic compounds First production units of the MS9 double-focusing, high resolution mass spectrometer have begun to leave Associated Electrical Industries' Manchester works. Designed specifically for high resolution studies of organic compounds, it has a guaranteed resolving power of 10,000, most likely will do "much better," the British firm says. With it, the chemist can measure mass, pinpoint structure more positively than he can with instruments of lower resolving power. The new model gives the organic chemist a tool that can do what formerly took teams of chemists operating custom units, AEI claims. The MS9, AEI's latest mass spectrometer, adds to an already impressive line. Early last year, the company introduced its MS7 double-focusing, spark source unit for trace solids analysis and its MS4 respiratory analyzer (C&EN, Feb. 13, 1961, page 55). And at the end of the same year, it brought out the MS 10—a low-priced ($4700 in the U.S.), kit-type instrument designed to be built into experi-
ments. AEI also makes four other models. Price of the MS9 in the U.S. is about $130,000. Picker X-Ray handles the unit in the U.S., along with AEI's other mass spectrometers. AEI says the new instrument has stirred up a lot of interest, pulled in a number of orders before the first demonstration. The new spectrometer sports, besides high resolving power, other impressive statistics: precision of mass measurement—at least 1 part in 100,000; accuracy—at least 2 parts in 100,000; scanning time—varies with application. Typical fast scans at a resolving power of 1000 takes about 10 sec. Uses. Main use of the MS9 is in precisely determining molecular weight from parent peak spectra and in analyzing structure. With the new instrument, the organic chemist can measure mass accurately to the third decimal, roughly to the fourth. He can thus distinguish between multiplets differing only slightly in mass. Similarly, he can precisely measure the mass of fragment ions and estab-
SAMPLE SYSTEMS. Two sample inlet systems are shown here. The one on the left with the glass flask is the cold inlet system, on the right is the hot valve system 64
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lish their composition. This in turn can help shed light on structure of the parent molecule, since groups of atoms tend to break off as whole units under electron bombardment. The MS9 may also find use in quantitative organic analysis where complex mixtures—lubricating oils, for example —demand high resolution, Dr. J. D. Waldron, chief engineer of AEFs scientific apparatus department, told, the 2nd ILMAC conference in Basle, Switzerland, recently. He cites mixtures of alkyl benzenes and benzothiophenes, which have the same molecular weight. They can't be separated in a complex mixture by conventional single-focusing mass spectrometers. But high resolution mass spectrometry shows promise. Key to the MS9 , s high resolving power is double focusing: In addition to the usual magnet analyzer, it has an electrostatic analyzer. It thus focuses for energy as well as for velocity. Radius of the electrostatic analyzer is 15 in., while that of the magnet analyzer is 12 in. The angle of both sectors is 90°. Design is the Nier-Johnson type. Although AEI is guaranteeing a resolution in every-day use of at least 10,000, it has obtained much higher values. For example, in a parent peak spectrum of a mixture of 1-methoxyand 1-4, diamino-anthraquinone, mass difference between parent ions was only 0.0112 in 238. This corresponds to a resolution of about 22,000. Variable Resolution. But the MS9 can also operate at lower resolving power, Dr. Waldron points out. Both source and collector slits can be adjusted by calibrated micrometers from outside the vacuum. The source slit can be varied from 0.003 to 0.0003 in. The collector slit can be adjusted from 0.030 to 0.0003 in. With these adjustments, resolving power can be varied from about 500 to more than 10,000. Thus, the operator can scan the whole'mass spectrum rapidly at relatively low resolving power (1000 to
ON THE MOVE WITH
In 1947, Royal China Company took a plunge • • •
They "gambled" an increase in raw material costs to replace a costly-to-operate wet clay preparation plant with a Simpson Mix-Muller. Air-floated clay, necessary for the dry mix process, then cost 25% more than the raw clay used for wet processing. By 1948, Royal had realized savings amounting to $2.41 per ton of material produced and saved floor space worth a cool $25,000! By 1960, when Royal replaced a second wet process (shown above—inherited in an expan-
sion move) nearly every China and Pottery plant in the U.S. had followed their lead...and the price of air-floated clay had been reduced through mass production economies. The opportunity for savings such as these are built-in to any liquid/solid or solid/solid blending process. And today you don't have to take a "plunge" to realize them. Just write for the Handbook on Mulling or for details on a laboratory mulling test for your materials . . . in a Simpson Mix-Muller.
a Write for your Handbook on Mulling
SIMPSON
NATIONAL ENGINEERING C O M P A N Y
DIVISION
6 4 3 M A C H I N E R Y HAUL B U I L D I N G
CHICAGO 6, ILLINOIS C & E N 65
THE GALLIC TOUCH Tons of Mallinckrodt h i g h - p u r i t y gallo-tannins provide t h e touch of elegance in dyeing furs and fashionable fabrics . . . work t h e i r m o r d a n t magic in dyeing leathers. F r o m clear headgear for j u n i o r spacemen to clarifying heady wines, a m y r i a d of products bear t h e gallic touch of this Mallinckrodt family of gallo-tannins.
A t Mallinckrodt there's a wealth of p u r e and applied knowledge available to you on t h i s molecule. If your product of today—or t h e f u t u r e — can profit from the gallic touch, w r i t e for additional information on gallo-tannins. I n d u s t r i a l Chemicals Division, Mallinckrodt Chemical Works, St. Louis 7, Missouri. LINKING CHEMISTRY TO INDUSTRY
MALLINCKRODT CHEMICAL WORKS St. Louis • New York • Montreal 66
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1962
2000), then slowly scan portions of special interest at the highest resolving power. There's no need to "waste" resolving power. This is important, since scanning time increases and instrument sensitivity falls off with increasing resolution. Ion source is the electron bombardment type. Mass range of the MS9 is 2 to 800 at the full ion accelerating voltage of 8 kv. But reducing voltage extends the range. At 2 kv., for instance, the upper limit is 3200. Actually, Dr. Waldron says, in a correctly designed instrument, it's not the spectrometer itself that limits mass range. The problem is introducing the sample. The sample system must cover a whole range of gases, liquids, and solids of widely varying volatility. Three independent sample systems are available in the MS9. One is a conventional cold inlet system for gases or volatile liquids. For vaporized liquids or solids, a hot valve system that can be heated to 350° C. also comes with the instrument. And AEI has also provided for a third, direct-injection sample inlet system. A bolted access port in the source housing gives line-of-sight entry into the ionization chamber. Through this port, the operator can inject samples directly into the source when performing experiments on direct evaporation of solids or when studying photoionization or free radicals. A vacuum lock allows the sample chamber to be pumped down to roughing pressure separately, thus leaving the rest of the vacuum system undisturbed. There are two independent final collector systems. The primary collector consists of an adjustable slit (0.030 to 0.0003 in.) mounted on the principal axis and an electron multiplier detector. This detector feeds an electrometer amplifier with 987r response time of 0.05 sec. The primary collector is for high resolution work or for fast scans at low resolution. The auxiliary collector has an adjustable slit (0.002 to 0.016 in.) mounted slightly off the principal axis but in the focal plane. This collector is for routine, low resolution scans up to mass 800 or for calibrating the electron multiplier. A monitor collector is located between the analyzers. It intercepts about half of the ion beam before there has been any separation and gives a measure of beam intensity. Both source and analyzer sections
THE RIGHT STEAR F r o m coating paper for gift w r a p pings to finishing f u r n i t u r e with a flair, i n d u s t r y t u r n s to t h e specialized experience of Mallinckrodt for t h e r i g h t s t e a r on stearates . . . in waterproofing, shell molding, coating, finishing and powder metallurgy. Tons more of magnesium, zinc, aluminum and calcium stear a t e s from Mallinckrodt make a demonstrable difference in phonog r a p h records, gun powder, fishing line, t i r e s and crayons.
S t e a r a t e technology at Mallinckrodt offers you unequaled production and research assistance. If you are looking for t h e r i g h t s t e a r t h r o u g h a maze of product p a r a m e t e r s , w r i t e now for additional information on stearates t o : Industrial Chemicals Division, Mallinckrodt Chemical Works, St. Louis 7, Missouri. LINKING CHEMISTRY TO INDUSTRY
MALLINCKRODT CHEMICAL W O R K S St. Louis • New York • Montreal
RIGHT IN ANY ELEMENT The many mercury compounds from Mallinckrodt are today serving the needs and desires of man in every element—air, water, earth and the far reaches of space. Some are used in carbon brushes of home power tools and intensifiers in film. Others preserve wood, protect paint from fungi and yard umbrellas from mildew. On center stage are the mercury compounds used in batteries that power the portables that bring in your favorite radio fare from across town—or halfway across the world via active communications satellites.
Whatever environment you are involved with, from elementary to elaborate, Mallinckrodt mercurial specialties can often provide a profitable answer. If you seek a mercurial answer to a specific problem, write for additional information on m e r c u r y compounds. I n d u s t r i a l Chemicals Division, Mallinckrodt Chemical Works, St. Louis 7, Mo. LINKING CHEMISTRY TO INDUSTRY
rJfaffindmtf MALLINCKRODT CHEMICAL WORKS St. Louis • New York • Montreal
have separate vacuum pumping lines. The narrow source slit is the only connection between the two regions. When the slit is widest (0.003 in.), the pressure in the analyzer is at least 10,000 times less than that in the source. This system is designed to curb contamination of critical surfaces by organic compounds. So far, Dr. Waldron says, a similar system in the MS8, prototype of the MS9, has worked well. It hasn't been necessary to clean the electrostatic analyzer plates in four years of operation. Cooperative Effort. The MS9 is a direct outgrowth of the MS8, which was developed by AEI for Dr. J. H. Beynon of Imperial Chemical Industries' dyestuffs division. The MS8 is a one-of-a-kind unit built by AEI to Dr. Beynon's requirements. It was designed to exploit Dr. Beynon's technique of correlating structure and mass spectra. Dr. Beynon and his group have been using the MS8 since 1957, with one year of joint operation at AEI. According to A. E. Williams, ICI technical officer and assistant to Dr. Beynon, the MS8 will resolve to one part in 10,000 "comfortably/' Dr. Beynon's interest in harnessing the mass spectrometer to organic chemical analysis goes back some 10 years. In 1953, he decided to see to what limits he could push his spectrometer, which he and his group had built from a published design. Although double-focusing instruments existed, they were used for fundamental mass measurements, Mr. Williams says. None existed for analysis. Dr. Beynon's home-made unit had a nominal resolving power of about 600, but he found that by closing down the movable exit slit, he could get high resolution with mass precision of 20,000. Later, he increased this to 100,000 by using the rectified form of a plot of the derivative of the spectrometer output. But he could work only with parent ions. His singlefocusing instrument couldn't focus fragment ions with their larger energy spread. Meanwhile, the group was also busy compiling a mass table of the precise molecular weights of various combinations of carbon, hydrogen, nitrogen, and oxygen. The table covers masses to 250 has been published in Dr. Beynon's book, "Mass Spectrometry and Its Applications to Organic Chemistry." They have since extended the table to include masses to 500.
P-N-P . . . CALL LETTERS OF PROGRESS Wherever the nanosecond pulse of electronics leads next in our probing of space and matter, chemicals from Mallinckrodt will continue to play a vital role. More than a dozen controlled-purity chemicals serve the transistor alone, including the silicon of which it's made. Chlorides, carbonates, sulfates, alkalies and acids by the score are essential to all components: tubes and their sockets, capacitors and resistors, printed circuits, f errite cores, wires and batteries.
Nowhere can the precise purity standards required by the electronics industry be better met than at Mallinckrodt, where nearly a century has been devoted to acquiring the skill. If P-N-P are your call letters, write for additional information on electronic chemicals to the; Industrial Chemicals Division, Mallinckrodt Chemical Works, St. Louis 7, Missouri. UNKING CHEMISTRY TO INDUSTRY
MALLINCKRODT CHEMICAL W O R K S St. Louis • New Y o r k • Montreal DEC.
17,
1962
C&EN
67
DOUBLE-RAM EXTRUDER OPERATES CONTINUOUSLY
NEW!! PORTABLE
Extrusion cylinder and ram-
LAB RACK •C*
v
Electric heatert
m
4? f v r \
DU block
Ram Extruder Operates Continuously Bell Labs designs double ram plastics extruder which overcomes disadvantages of older machines
MODE L
LR 3002
v
Just ONE of a COMPLETE LINE of PORTABLE SYSTEMS from PENN-CHEM including: • Portable Vacuum Assembly Carrier • All Purpose Carriers • Portable Lab Racks • Portable Towers • Cantilever Carriers • Glassware Carriers
These hardworking carriers put virtually every laboratory operation ON WHEELS. VERSATILE? Sets up for scores of uses • . • • Vacuum Pumps & Accessories • Distillation Columns & Accessories • Column Chromatographic Equipment • Gas Analysis Apparatus • Reaction Set-ups • Filtration Equipment, etc. For catalog and prices contact your laboratory supply dealer or write Dept. B-12.
sssBssiaasssa 232-238 N. MARSHALL STREET LANCASTER, PENNSYLVANIA
68
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Bell Telephone Laboratories has developed a reciprocating, ram-type, plastics extruder. Robert Westover of Bell Labs says the device overcomes the usual disadvantages of ram extruders. These include discontinuous flow, prohibitive heating times, and gas entrapment. Mr. Westover detailed the extruder at the winter meeting of the American Society of Mechanical Engineers in New York City. Mr. Westover points out that the new extruder provides high pressures with independent control of temperature and pressure, fast equilibrium response to change in extrusion pressure, and little shear degradation of material. In the experimental model extruder, Mr. Westover explains, the flow rate at the die is controlled by the flow properties of the material in the region of the die. Flow rate is also controlled by pressure exerted by either one or both of two rams (one-inch diameter). These rams are placed above the extruder. Hydraulic pistons provide the rams with their driving force. Extrusion pressures of up to 12,000 p.s.i. can be obtained. Band heaters around the head, die block, and cylinders surrounding the two rams provide a near-constant temperature. Since retention time in the heat is too short to provide adequate heating of the material, stock material is preplasticized or preheated before entering the head. Preheated stock material is fed into the head by two injection machine cylinders and ram combinations.
Valving Does the Job. The heart of the extruder, Mr. Westover says, is the valving arrangement. Here the discharging cycle of one extrusion ram begins just before the other has exhausted its charge. Timing and direction of flow of material from the preplasticizing cylinders are also controlled by the shuttle valve system. While the shuttle valve is in the extreme left position, the left-hand extrusion ram has delivered and nearly exhausted its charge. The right-hand extrusion ram is forced to retract and takes on the charge of material from the right-hand plasticizing cylinder. When the material is forced from the plasticizing cylinder it moves the slide valve to the left. Valve ports are arranged so that the left extrusion channel starts to open before the right one begins to close. Finally, in the extreme left position a path is provided for a new charge from the plasticizing cylinder to flow through the conical hole in the end of the valve and from there through a small hole into the edge of the extrusion cylinder. In jetting through this small hole, the material undergoes its only high shear rate within the extruder. Shear rate can be adjusted by controlling the injection pressure or dimensions of the hole, Mr. Westover says. By jetting the fresh charge of material into the extrusion cylinder at the edge, this new material gets past the remainder of the previous charge so that the older material is the first to be extruded on the next stroke of the extrusion ram. Mr. Westover points out
that the design of the extruder eliminates hang-up of material and thus prevents degradation. Maximum output of the ram extruder has gone as high as 20 lb. per hour, the Bell scientist says. Extrusion pressures ranged as high as 12,000 p.s.i. And temperature range is limited only by the polytetrafluoroethylene O-rings used as seals on the extrusion ram, he adds. Higher extrusion temperatures are possible with other ring materials.
BRIEFS An electrically heated evaporator, designed to concentrate mildly radioactive liquid waste, has been developed by Barnstead Still and Sterilizer Co., Boston, Mass. The still is designed to concentrate the volume of shower and laundry drainings, process rinse water, and other large volumes, the firm says. Liquid wastes are fed continuously and the unit is equipped with suitable safety and operation controls. E 30
POTASSIC POTPOURRI Spinning tires, soaring satellites, soft-step carpets—all depend on Mallinckrodt potassium compounds. Light a cigarette or put out a fire —potassium salts do the job behind the scenes. Take a picture and potassic genies are busily working away in the flash bulb, film and paper—even in modern "instant" photography. Whether it's instant or sustained improvement in performance, some Mallinckrodt potassium compound can do the job.
Mallinckrodt has a way with potassium compounds, backstopped by solid technology. If profit is your problem, this potassic potpourri may hold the answer. For additional information on potassium salts write to: Industrial Chemicals Division, Mallinckrodt Chemical Works, St. Louis 7, Missouri. UNKING CHEMISTRY TO INDUSTRY
Long counter for fast neutron flux measurements has been introduced by Texas Nuclear Corp., a subsidiary of Nuclear-Chicago Corp., Chicago, 111. The instrument, designated Mode] 9100, is calibrated to measure neutrons with energies ranging from 500 k.e.v. to 15 m.e.v. E 31
Universal manipulator for high vacuum systems has been developed by MRC Mfg. Corp., Orangeburg, N.Y. According to the firm, the manipulator, designated MRC V4-120, is useful in getting into a system to grasp, lift, turn, or move an object without disturbing the vacuum. The unit is designed for use in a vacuum of 10 -7 torr, the firm adds. E 32 Porous ceramic disks of Filtros material are offered. The media are said to ensure pure, dry, oil-free compressed air and gases. The high porosity and uniformity of this media will trap and filter out all dirt particles, scale, oil, condensed moisture, and other foreign matter, according to Filtros, Inc., East Rochester, N.Y. E33
CHEMICAL TOWER OF BABEL The world of gifts creates a nearly endless list of processing requirements . . . calling for chemicals so diverse they don't speak the same language. At Mallinckrodt you find the chemical array to match that diversity. Initiate or inhibit a reaction. Regulate particle size. Control setting time. Catalyze. Processing problems that may appear unrelated . . . can have a common denominator : Mallinckrodt!
For here is nearly a century of experience in making specialized chemicals of dependable quality, consistent purity. If your product of today—or the future—presents an enigma, indicate where our assistance and high volume custom manufacturing can make a contribution. Write now to: Industrial Chemicals Division, Mallinckrodt Chemical Works, St. Louis 7, Mo. UNKING CHEMISTRY TO INDUSTRY
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ECONOMY—1 pound of Lupersol 11 is equivalent to at least 3 to 6 pounds of a conventional initiator, such as lauroyl peroxide. Shorter induction times are a noteworthy feature of Lupersol 11's higher reactivity which makes possible shorter conversion cycles. IMPROVED POLYMER PROPERTIES — as an efficient source of aliphatic free radicals at low temperatures, Lupersol 11 produces resins with outstanding heat and light stability, excellent electrical properties, increased linearity and higher molecular weight. A major decom-
position product is the t-butyl radical which, although efficient, minimizes hydrogen abstraction from t h e polymer chain and resultant branching. CONVENIENCE—Being a liquid, Lupersol 11 is easy to meter and disperse. Although safely handled at room temperature, moderate refrigeration is required to preserve its activity in storage. Shipment will be made by Lueidol's refrigerated trucks to most areas east of the Rockies.
WALLACE &TIERNAN INC. Write for Data Sheet
70
C&EN
LUCIDOL DIVISION
1 7 4 0 Military Road Buffalo 5, N e w York
(Princeton), Ltd., Princeton, N.J. The bath is suggested as a convenient way of heating materials to 350° C. The Techam fluidized bath has two electrical heaters and a stainless steel liner. E 34
Laboratory mixer with V 50 hp. electric motor is offered by Eclipse Air Brush Co., Newark, N.J. The unit has an integral speed control. Electrimix Model 50-4050 is engineered for cool running and quiet operation, according to the company. E 35
Steam-jacketed
safety
relief
The valve assures free flow of viscous materials at ambient temperatures, according to the firm. E 36
Compact recording controller is available from Partlow Corp., New Haven, Conn. As many as three control switches can be included. The unit also features an optional inkless marking system. The unit was primarily designed for use in transit refrigeration, but is available for standard industrial uses, the company says. E 37
Further useful information on keyed Equipment items mentioned is readily available . . .
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available from Farris Engineering Corp., Palisades Park, N.J. The valve is designed for use where temperature of process fluid must be maintained.
Use handy coupon on page 72
December 17,1962
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. (Please fill out coupon completely.)
Name:
I I j |
how to cultivate taste You can't sweet-talk contaminated gas out of your product or process. Soda water, hydrogenated foods and dry ice producers learned long ago that activated carbon gas purification is an essential step in producing a palatable product. How clean are your bubbles?
how to paint out the smell
M
Filters, fabrics and containers do double duty when coated with activated charcoal paint. Sprayed or brushed on it adsorbs odors instead of producing them. Can be washed off after saturation. Try a quart or a tank car.
Company: O OT
Street: — Zone-
City
State
activated carbon
Your Title: Your Function (Check One): 1 2 3 4 5
• • • • D
Corporate Management Technical Management Product Research Product Design & Development Process Research
6 7 8 9 10
• • • • •
Process Design & Development Production—Processing Purchasing Analysis—Testing Consulting
CLIP COUPON—Fold along this line—fasten (staple, tape, glue) MAIL
Your Industry:
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Petroleum Ref., Asphalts, Lubricants Rubber; Plastic Products Leather & Leather Products Stone, Clay, & Glass Products Primary Metal Industries Fabricated Metal Products Machinery & Equipment Transportation Equipment Instruments Education
We supply a complete line of activated carbons for every purpose; design and prefabricate complete purification, separation, and recovery systems to meet your particular needs. Write for Bulletin 60-9D and recommendations on your specific application. Barnebey-Cheney, Columbus 19, Ohio.
Barnebey Cheney DEC.
17, 1 9 6 2 C & E N
71
