INSTRUMENTATION - Analytical Chemistry (ACS Publications)

Publication Date: July 1954. ACS Legacy Archive. Cite this:Anal. Chem. 26, 7, 31A-34A. Note: In lieu of an abstract, this is the article's first page...
0 downloads 0 Views 2MB Size
INSTRUMENTATION A n a l y t i c a l Instrument Clinic will offer demonstrations a n d lectures on latest a n d most a d v a n c e d a n a l y t i c a l instruments

H. ONPCeEt emr soor ne wfore a r ec oimn dpel ebttee d itnof oAxel rmation regarding the Annual Analytical Instrum e n t Clinic. I t h a s a d d e d significance t h i s t i m e b y v i r t u e of i t s i n t e r n a t i o n a l aspect. T h e I n s t r u m e n t S o c i e t y of A m e r i c a a n n o u n c e s p l a n s for t h e T h i r d A n a l y t i c a l I n s t r u m e n t Clinic t o b e h e l d S e p t e m b e r 13, 14, a n d 15 in c o n j u n c t i o n w i t h t h e First International I n s t r u m e n t Conference a n d E x h i b i t t o b e held a t P h i l a d e l p h i a , S e p t e m b e r 13 t o 2 5 , 1954. T h e clinic is a l e c t u r e a n d d e m o n s t r a t i o n course o n t h e l a t e s t a n d m o s t a d vanced analytical instruments. I t is p l a n n e d for t e c h n i c i a n s , e n g i n e e r s , p h y s icists, a n d c h e m i s t s w h o a r e u s i n g , or cont e m p l a t e using, t h e s e i n s t r u m e n t s . It will b e especially v a l u a b l e for g r a d u a t e s t u d e n t s in c h e m i s t r y a n d p h y s i c s . T h e 3-hour session on e a c h i n s t r u m e n t will b e c o n d u c t e d b y t w o or m o r e e x p e r t s a n d will cover t h e t h e o r y of t h e i n s t r u m e n t , electronic, o p t i c a l , a n d m e c h a n i c a l design f e a t u r e s as well as d e t a i l s of application. A d v a n c e r e g i s t r a t i o n will b e r e q u i r e d . A n y n u m b e r of sessions, u p t o five, m a y b e a t t e n d e d . T h e sessions o n e a c h i n s t r u m e n t will b e s m a l l a n d will b e r e p e a t e d u p t o a m a x i m u m of five t i m e s . F o r registration form a n d further information w r i t e t o Axel H . P e t e r s o n , M e l l o n I n s t i t u t e , 4400 F i f t h A v e . , P i t t s b u r g h 13, P a . W e a r e listing t h e p a r t i c i p a t i n g c o m p a n i e s ' o u t l i n e s of t h e p r o g r a m w h i c h t h e y will p r e s e n t , a n d also t h e p a p e r s t o b e p r e sented a t t h e analysis instrumentation sessions. X-Ray Q u a n t o m e t e r s , Applied Research Laboratories I. Introduction A. Principles of fluorescent x-ray _ analysis. B . F a c t o r s affecting limits of detectability (qualitative analysis). C. F a c t o r s involved in q u a n t i t a t i v e analysis. II. Instrumentation A. X - r a y tubes and power supplies, requirements for fluorescent x-ray analysis. B . Radiation analyzers. 1. Description and applications of nondispersive analyzers. VOLUME

2 6,

NO.

7,

JULY

1954

III.

IV.

V.

Crystal spectrometers, dis cussion of flat and curved crystal t y p e s . 3. Energy analyzers, brief discussion of m e t h o d and a p plicability. X - R a y Quantometers A. Detailed description of x-Ray power supply. B . Detailed description of spectrometers used. C. Detailed description of receivers and recording circuits. Quantitative Analysis with t h e X - r a y Quantometer A. Discussion of sampling problems. 1. Metallic samples. 2. Nonmetallic samples. B . Determination of operating conditions. 1. So urce parameters. 2. Spectrometer adjustment, interferences, filtering. 3. Circuit adjustments, scale spread. C. Preparation of working curves. 1. Sample systems. 2. Multicomponent systems. D . Precision and accuracy. Special Problems A. Coating gaging problems, method, applicability. B. Absorption analysis.

by Ralph H. Millier

2.

Littrow-Echelle Spectrograph, Bausch & L o m b Optical Co. I. Introduction A. Advantages of high resolving power and high dispersion in spectroscopy. B . Principle of t h e Echelle. C. F r e e spectral range a n d cross dispersion. D . Properties of an Echelle. I I . Littrow-Echelle Spectrograph A. Design considerations. B . Operation as a L i t t r o w spectrograph. C. Operation as an Echelle instrument. I I I . Discussion of other Echelle instruments A- Echelle a t t a c h m e n t . B . WadsworthEchelle spectrograph. C. Other Echelle spectrographs. IV. Applications for Littrow-Echelle spectrograph A. Complex spectra. B . Isotopic analysis. C. Zeeman p a t t e r n s and hyperfine structure. D . Unsuspected interferences. E . Separation of overlapping lines. V. Demonstration and discussion Infrared Spectrophotometers for Research a n d Product Control, Beckm a n Instruments, Inc. I . Introduction A. Infrared in research and p l a n t trouble shooting. B . D e t e r m i n a t i o n of stream and atmospheric pollution. C. P r ocess control.

II.

III.

IV.

I n s t r u m e n t design features A. Optics. B . Electronic m e m o r y system. C. Purge system t o remove b a c k ground. D . Micro-optics for micro samples or small K B r disks. E . Slit drive system. Operational demonstrations A. Controls and functions. B . Actual sample runs d e m o n s t r a t e ing quality control. C. Pro c ess c ontrol. Discussions

Process Monitoring Mass Spectrometers, Consolidated Engineering Corp. I. Introduction A. Principle of magnetic separation of electrically charged particles utilized in analytical instruments. B . Application of t h e principle in a continuous process monitoring mass spectrometer. I I . Design features of major c o m p o n e n t s , discussion and display A. Analyzing unit, t h e D i a t r o n . B . V a c u u m system. C. Sampling systems, batch t y p e and continuous. D . Amplifying and recording systems. E . Automatic peak selector. I I I . Operation and Maintenance I V . Performance D a t a A. Resolution and mass range. B . Analytical and monitoring capabilities. C. R a n g e of detection. D . Stability, sensitivity, and p a t tern. V. Application examples A. Analytical. B . Process monitoring and control. C. Leak detection. V I . D e m o n s t r a t i o n of actual operation A. B a t c h analyses. B . Continuous monitoring. V I L A more versatile process monitoring mass spectrometer utilizing a newly developed principle A. Principle of cycloidal focusing. B . Analyzing unit, t h e cycloidal tube. C. Application of principle in a continuous process monitor. V I I I . Performance D a t a A. Resolution and mass range. B . Analytical and monitoring capabilities. C. Range of detection. D . Stability, sensitivity, and p a t tern. I X . Application examples A. Analytical. B . Process monitoring and control. 31 A

UNLOCK the door to molecular secrets

INSTRUMENTATION

with High Resolution n-m-r S p e c t r o s c o p y

The Varian Model V-4300 High Resolution n-m.r (nuclear magnetic reso­ nance) Spectrometer has stirred the imagination of chemists everywhere. With this new instrument, signals from H 1 , F19, P31, B n , C13 and several other nuclei can be detected, revealing the occurrence of identical nuclei in different chemical environments. High Resolution iwn.r techniques permit rapid and completely non-destruc­ tive study of small liquid samples, including melted solids and liquefied gases. Outstanding applications include: • Identification of functional groups • Assignment of structural formulas » Analysis of multi-component mixtures

THIS IS N-Nl-R AT WORK (Number 4 of α «·"«) 1K1 D Q RAPID QUANTITATIVE ANALYSIS OF H.O IN D 2 0 INTERPRETATION DATA Samples: (A) 5 > H , 0 in D,0 (control)

,HH2OinD (B)1 (B) 1% 00(con (control)r 20 in D22

^ K W ^ S f f i g S ic) 3.4* H20 in D20 (unknown) ^ = % « ^ » ^ Volume: .03 cc. » • ; , * £ Γ eBÏÏ.™%.SS» Signals observed: Η' ΗϊΞ^ο^ο^» Frequency: 30 mc ° f ° ° ^ = ) | S J,Ç«,«,, ,.gn.| ^SSrni.ii.uss/sec.

»

»

A

r^j^l

CONTROL SAMPLE A

,

Ion Resonance Mass Spectrometer, General Electric C o . I. Introduction A. Principles of resonance phenomena utilized. B. Development of resonance equations and discussion of accelerating potentials. II. Design features of the mechanical components, inspection and discussion A. Ion resonance tube. B. Vacuum system. C. Sample system. III. Theory and operation of electronic components A. Direct-coupled amplifier. B. Oscillator. C. Emission regulator. D. Vacuum metering panel. IV. Operation and maintenance discussion V. Performance data A. Resolution. B. Sensitivity. C. Analytical ability. D. Cracking pattern stability. E. Examples of applications. VI. Operation Demonstration. Nondispersion Infrared Analyzers, Liston-Becker I n s t r u m e n t Co. I. Introduction A. Principles of infrared analyzers. B . History of development of nondispersion analyzers. 1. Negative type, development in this country. List of manufacturers making this type, with distinctive characteristics. 2. Positive type, development in Europe. List of current manufacturers with characteristic properties. C. Characteristic differences and advantages of each type. II. Typical performance possible with nondispersion analyzers A. Maximum sensitivities obtainable. B. Resolution and discrimination realized on difficult problems. C. Stability realized. Installation problems III. A. Obtaining representative samples. B. Sampling time and flows. C. Filtering and conditioning of samples. IV. Construction of Liston-Becker analyzer A. Sample cells. B. Optical window materials. C. "Unitized" construction. D. Provisions for servicing. V. Typical applications In addition to the lecture, an operating demonstration will be given and slides will be used to illustrate various points. Nuclear M a g n e t i c Resonance ( n - m r) Spectrometer, Varian Associates I.

FOR THE COMPLETE STORY . . . On Varian's Model V-4300 High Resolution n-nvr Spectrometer, write to the Special Products Division for: • • • T H E

Technical Information Bulletins Data Sheets n-nw Table

M A R K O F

II.

L E A D E R S H I P

VARIAN a s s o c i a t e s PALO

A L T O

2,

C A L I F O R N I A

For further information, circle number 32 A on Readers' Service Card, page 39 A

32 A

III.

Introduction A. Fundamental principles of n-m-r. B. Historical background and development of applications. C. Various forms of n-m-r spectroscopy; description of and distinctions between variable frequency, spin echo, and high resolution. D. Typical n-m-r spectra. Details of high resolution spectrometer A. Probe. B. Radio-frequency unit. C. Sweep unit. D. Signal display units. E. Maintenance. Details of associated magnet system A. Over-all design considerations. B. Field homogeneity. C. Field stability. D. Maintenance.

ANALYTICAL

CHEMISTRY

NOW! A NEW CONCEPT IN GAS FLOW COUNTERS

INSTRUMENTATION IV.

for maximum efficiency with carbon 14 and other soft beta emitters featuring windowless operation for greatest sensitivity or "Micromil"* window operation for the newest and best method of counting soft beta radiation. Newest—because the exclusive "Micromil" window is so thin that it reduces the count rate for carbon-14 by less than 20%. Better—because common windowless counter problems (charge effects, chamber contamination, moisture accumulation) are completely avoided. Model D47 may be used with the automatic sample changer or chromatographic strip scanner—is the most versatile gas flow counter ever produced!

Operating techniques a n d demonstration A. Sample handling. B . Reference compounds. C Chemical shift measurements. D . Advanced techniques.

Preliminary Program of Instrumentation Sessions

Tuesday, September 14, 9:30 A.M. Raman

Spectrometer

Available C o m p o n e n t s .

Write for Model D47 specifications

ARCHIE

PEABODY,

Mervyn

Instruments,

Wednesday, September 15, 9:30 A.M. A N e w Mass Spectrometer.

T. H. M C -

L A R E N AND W . C . W I L E Y , R e s e a r c h L a b o r a -

tory, Bendix Aviation Corp., Detroit, Mich. An R . F . Accelerator for Leak Detection. DONALD G. TIPOTSCH, Beckman Instruments,

Inc., Pasadena, Calif. An R . F . Linear Decelerator M a s s SpecWALTER

DONNER,

Beckman

I n s t r u m e n t s , Inc., Pasadena, Calif. Wednesday, September IS, 2:30 P.M. Performance of a N e w Monitor M a s s Spectrometer. H . F . W I L E Y , Consolidated Engineering Co. Operation a n d Maintenance of I o n R e s o nance Mass Spectrometer. W . A. M O R G A N , General Electric Co. An R F Mass Spectrometer Utilizing Linear Accelerator. M . K . TESTERMAN, University of Arkansas, Fayetteville, Ark. Friday, September 17, 9:30 A.M. Nuclear Magnetic Resonance. I t s P r i n ciples a n d I n s t r u m e n t a t i o n . J A M E S N . SHOOLERY, Varian Associates, 611 Hansen Way, Palo Alto, Calif. Some Chemical Applications of Nuclear Resonance.

JOHN

P.

O'MEARA

AND W . ROLLWITZ, Southwest Research I n stitute, San Antonio, Tex. D e t e r m i n a t i o n of Molecular S t r u c t u r e Fluorocarbons b y Nuclear Magnetic R e s onance. D . G. W E I B L E N , Minnesota M i n ing & Manufacturing Co., St. Paul, M i n n . Some Chemical Applications of Nuclear Magnetic

Nuclear Instrument and Chemical Corporation, 223 West Erie Street, Chicago 10, Illinois

nuclear

from

Working Surry, England. Universal Spectrophotometer designed for Laboratories a n d Industrial C o n t r o l purposes, Needing High Accuracy. FRANCOIS D E S V I G N E S , Paris, France.

Magnetic

*Trademark

Assembled

H E N R Y LAWRENCE,

American C y a n a m i d Co., B o u n d Brook, N. J . A N e w G r a t i n g Infrared Spectrometer.

trometer.

. . detects all soft or hard ionizing radiations . . converts from windowless to thin window in seconds . . permits both geiger or proportional counting . . bubbler and valve adjustments completely eliminated . . extremely low background . . now in production

Analysis

- chicago

Resonance.

JOHN

Massachusetts I n s t i t u t e Cambridge, Mass.

of

S.

WAUGH,

Technology,

Monday, September 20. 9:30 A.M. Application of Radioactive Gaging t o Process Measurement a n d Control. P H I L I P E . O H M A R T AND H . L. C O O K , J R . , T h e O h m a r t

CHICAGO NEW YORK LOS ANGELES DALLAS HOUSTON SILVER SPRING, MD.

Corp., Cincinnati, Ohio. Redox Potential for Industrial

Control.

D A V I D H . F U L L E R AND J O H N G.

DOBSON,

T h e Foxboro Co., Foxboro, Mass. A C o n t i n u o u s Analyzer for Oxygen in T r a c e Quantities. Louis THAYER AND M I C H A E L C Z U H A , J R . , A. O. B e c k m a n , I n c . ,

Pasadena, Calif. A n I n s t r u m e n t for Continuous D e t e r m i nation of Dissolved Oxygen Based o n Paramagnetism.

ALFRED

D.

ROBINSON

AND

L o u i e T H A Y E R , A. O. Beckman, Inc., P a s a dena, Calif. Monday, September 20, 2:30 P.M. Viscosity Control with Bendix Ultraviscoson. G. J . R O S E N B L I T , Bendix Aviation Corp., Cincinnati, Ohio. An Industrial Rotational Viscometer a n d I t s U s e with Materials of Varying Density. R. A. M I N A H D , Brookfield Engineering L a b oratories, Inc., Stoughton, Mass. N e w T y p e s of Photoelectric Measuring Devices.

Fir further Information, circle number 34 A on Readers' Service Card, page 39 A

34 A

BRUNO LANOE,

Berlin-Zehlendorf,

H e r m a n s t r , 14/18, Berlin, Applications of Flow Turbidimeters in Process LOR FLETCHER, Beckman Fullerton, Calif.

Germany. Colorimeters a n d Industries. T A Y Instruments, Inc.,

ANALYTICAL

CHEMISTRY