REPORT FOR ANALYTICAL
CHEMISTS
The Availability of Standard Reference Materials THE RAPID GROWTH of n e w W ITH instrumental analytical tech-
niques in the last two decades, the need has arisen for a wider variety of reliable standard reference materials. There is a lack of samples of certified high purity. Along with the shortage of certified samples is the need for accurate data on pure compounds including physicochemical properties. These problems were among those discussed at the Symposium on Standard Reference Materials and the Symposium on National and International Standards held by the ACS Divisions of Analytical Chemistry, Chemical Marketing and Economics, and Industrial and Engineering Chemistry in cooperation with the ACS Committee on Standardization Relations at the 148th National ACS Meeting in Chicago on September 3. Twentyfive scientists representing industry, government agencies, academic institutions, and scientific associations took part in the symposia. Dr. F. D. Rossini of Notre Dame University reported to the Symposium on Standard Reference Materials on the two-day National Academy of Sciences—National Research Council on Reference Standards held June 22 and 23, 1959. Although this conference was held over five years ago, its conclusions and recommendations are equally valid today. Among the conclusions reached at this conference, Dr. Rossini noted, was that there is a lack of samples of certified high purity. Accurate data on basic compounds are needed, including physiochemical properties. Research investigations are hampered by lack of thermal, spectral, and physical data. Systematic study on pure compounds is needed with rapid publication of results. The biggest need may be a method for coordination of scientific efforts in establishing specifications for refer-
ence materials, the Conference participants felt. It was concluded at the Conference that a strong scientific program with great depth be established in the field of reference standards. Government, industry, and university scientists must all take part in order to make the program successful. I t was recommended that some existing organization should establish a permanent information center for compounds of certified purity. The establishment of a permanent central technical organization for the preparation, analysis, and certification of purity and to provide for compound distribution was recommended. I t was further recommended that the program on reference standards cover a broad spectrum of compounds, take cognizance of foreign countries, implement communication and exchange of ideas, and encourage research on the preparation and analytical examination of pure compounds. The proceedings of this conference are being reprinted and will be available from the Office of Technical Services. Dr. W. W. Meinke of the National Bureau of Standards and Chief of the Bureau's new Office of Standard Reference Materials discussed the standard reference materials program at NBS. The Bureau presently has available more than 600 standard reference materials as summarized in NBS Miscellaneous Publication 241 available from the Office of Technical Services. It is also working on the development of about 50 new ones and has on hand requests for the preparation of many others. The requests have always far exceeded the Bureau's capacity to produce and certify these materials. One of the main functions of the NBS Institute for Materials Research is to develop, produce, and
distribute standard reference materials which provide a basis for comparison of measurements on materials and aid in the control of production processes in industry. To help carry out this function the Office of Standard Reference Materials evaluates the requirements of science and industry for carefully characterized reference materials, and directs their production and distribution. Emphasis is given to providing NBS Standard Reference Materials (a) where attainment of needed accuracy of analysis or accuracy of measurement of characteristics is not economically or technically feasible elsewhere, and where such accuracy is generally important to users, (b) where industry-wide standards for commerce are needed from a neutral supplier who is not otherwise available, and (c) where continuing availability of highly characterized material from a common source is important to science or industry. NBS recognizes the need for broadening the present program on reference materials to include all types of well-characterized materials than can be used to calibrate a measurement system or to produce scientific data that can be readily referred to a common base. With this broadening, however, it still remains apparent that the demand for new standard reference materials will continue to far exceed the Bureau's capacity for development. Therefore, requests for new standard reference materials which will have limited use and for which the need is not very great will have to be passed by in favor of requests clearly showing a critical need. For determining which requests are to receive top priority, the Bureau will need the information supplied by industry, either through its own representatives or through interested VOL. 36, NO. 12, NOVEMBER 1964
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REPORT FOR ANALYTICAL CHEMISTS committees, such as those of the American Society for Testing and Materials, the American Standards Association, and the International Organization for Standardization. While the B u r e a u welcomes all requests for the development of new standard reference materials, it will help both the Bureau, and industry as well, if requests are accompanied by such information as will permit an assessment of the urgency and importance of proposed new reference materials, D r . Meinke pointed out. I n discussing future plans for the N B S Standard Reference M a terials Program, D r . Meinke said t h a t the N B S is actively working on standards for Mossbauer spectrometry. This technique, he pointed out, gives information on binding of atoms in molecules. T h e B u r e a u is calibrating a number of crystals of sodium nitroprusside. This work will hasten routine application of the Mossbauer Effect in analysis, Dr. Meinke believes. AMERICAN PETROLEUM INSTITUTE STANDARD SAMPLES
Manufacture of petroleum products and petrochemicals such as aviation gasoline and monomers for synthetic rubber requires careful analysis in research, A. J. Streiff of Carnegie Institute of Technology told the Symposium on Standard Reference Materials. Spectral measurements by infrared, ultraviolet, mass, R a m a n , and nuclear m a g netic resonance, together with gas chromatography, have become valuable tools for fast and precise analyses. T h e instruments developed for these purposes need to be calibrated, and calibration is dependent on the purity of standards from which it is determined. During World W a r I I , the American Petroleum Institute Research Project 6 on the composition of petroleum began to purify standard samples of hydrocarbons and to certify their purities in a joint effort with N B S . Since 1950 this activity has been a cooperative effort of the American Petroleum I n stitute (API) and the Carnegie Institute of Technology. All of this work has been consolidated into a 24 A
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single project designated A P I R e search Project 58 on the Synthesis and Purification of Standard H y drocarbons. T h e p a r t of the Project concerned with synthesis, directed by E. J. Eisenbraun, is located at Oklahoma State University; purification and certification of purity is directed by Mr. Streiff a t Carnegie Institute of Technology. S t a n d a r d samples of organic sulfur compounds and organic nitrogen compounds have been produced by A P I Projects 48 and 52, respectively, located a t the laboratories of the U. S. B u r e a u of Mines in Laramie, Wyoming, and Bartlesville, Oklahoma. A P I standard samples of 310 hydrocarbons, 38 organic sulfur compounds, and 9 organic nitrogen compounds m a y be purchased from the A P I Samples Office a t C a r n e gie Institute of Technology. These standards have certified purities. (The target is a purity of 99.9%.) T h e y are made available in units of 5 ml., completely degassed and sealed under their own vapor pressure in glass ampoules. Carbon number range of the hydrocarbons is C 4 to Ci8. Present emphasis is being placed on synthesizing and purifying new standard hydrocarbons in the C12 to C i 8 range. Some standard hydrocarbons used for checking instruments and techniques have recommended values of refractive index and density supplied with the samples. AVhen a hydrocarbon is purified, several hundred milliliters of m a t e rial of the very highest purity which can be produced is reserved for research measurements of needed physical, thermodynamic, and spectral data. These A P I research hydrocarbons are loaned to qualified investigators for a wide variety of measurements. T h e d a t a which are obtained on A P I research hydrocarbons can be found in the Tables of Selected Values of Properties of Hydrocarbons and Catalogs of Spectral D a t a of the A P I Research Project 44 which is located at Texas A&M University. Purification of A P I standard and research hydrocarbons is accomplished by the use of the following fractionating processes: high efficiency distillation, both regular
and azeotropic, liquid-solid chromatography, crystallization or zone refining, and formation of solid molecular compounds. Distillation is used most often, and a completely equipped laboratory for distillation containing 14 columns, each 20 feet in height, is p a r t of the facilities a t Carnegie Tech. Careful purification of hydrocarbons must be followed by equally careful determination of purity. Methods are used which measure quantitatively very small amounts of impurity. The purity of hydrocarbons which can be crystallized is determined by calorimetric cryoscopic measurements. For compounds which do not crystallize, the purity is evaluated from careful gas-liquid chromatographic measurement using capillary columns 20 to 600 feet in length with hydrogen flame detection. Continuing efforts to improve methods of purification and determination of purity ensure t h a t American Petroleum Institute standard and research hydrocarbons continue to be major chemical guidelines for research, development, and control. THE OAK RIDGE RESEARCH MATERIALS INFORMATION CENTER
One of the continuing needs in materials research is information on the availability of high quality research specimens whose purity or composition is precisely known, T. F . Connolly of Oak Ridge N a t i o n a l Laboratory told the Symposium on S t a n d a r d Reference Materials. Although a large number of interesting materials are produced by commercial, government, and university laboratories, open literature publications or sales catalogs seldom indicate the source and purity of starting materials, methods of further purification, crystal growth, and assay of the end product, Mr. Connolly pointed out. T h e Research Materials Information Center was established as a p a r t of the Pure Materials P r o gram of the Solid State Division of the Oak Ridge National Laboratory to collect and provide this information to both producers and users. T h e primary emphasis is on high
new
REPORT FOR ANALYTICAL CHEMISTS purity inorganic research materials (usually single crystals) such as metals, alloys, semiconductors, re fractory or insulating compounds, laser and optical materials, and magnetic materials. Structural materials, devices, and radioiso topes are not included, since these are covered by the Defense Metals Information Center a t Battelle Memorial I n s t i t u t e and the Iso topes Information Center a t Oak Ridge National L a b o r a t o r y . An aperiodic bulletin, newsletters containing selected articles on m a terials preparation and evaluation, and lists of available and desired materials are published and dis tributed to all participants in the program. No purchases, loans, or exchanges are handled directly. However, recipients of information are asked to notify the Center of results on a n y specific material in order t h a t its records can be ad justed accordingly. General searches of the entire collection for the purpose of re views are made on occasion, and the collection and searching mecha nism is available for use by visitors to the laboratory. W h e r e the searches turn out to be extensive and there is a possibility of their being of general interest, a record is kept of the references sent out. T h e lists are filmed and are then available as the core of future searches. Lists of references on ferroelectric materials (inorganic single crystals), iron crystals and films, and refractory metals and compounds have been compiled. E q u i p m e n t has been installed t h a t will conduct an automatic search for coded entries t h a t have been placed on film (including more than 1500 d a t a sheets). Requested material for which no information is available is also listed, and the requester notified if such material becomes available. Background information on m a terials is also collected and en coded. A list of more t h a n 300 coding terms has been established under such general categories as T y p e and F o r m of M a t e r i a l , C r y s tal Structure. Electrical Proper ties, Growth Techniques, etc. E a c h category is further divided into ad ditional coding terms. Open litera-
ture publications, company reports, abstracts, and preprints have been collected and coded; and the col lection contains about 9,000 docu ments on about 30 reels (100 ft. each) of 16-mm. film. E a c h reel can be searched for set of coding terms in about 15 seconds. Mr. Connolly emphasized t h a t close cooperation is required be tween the Center and those who analyze, grow, and characterize re search quality materials. The most immediate and continuing need of the Center is for completed d a t a sheets from all producers of such materials, and for a rapid notifica tion of any significant new result or development via internal reports, preprints, or personal communica tion.
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THE INTERNAL C O M P A N Y STANDARD
I n discussing t h e internal com p a n y standard, M . D . Cooper of General M o t o r s Research L a b o ratories pointed out t h a t it has been the practice of some companies to m a k e their company standards available outside of their own or ganizations. However, these are company s t a n d a r d s not -primary standards, Mr. Cooper emphasized. By definition, primary standards must be certified by a recognized standardizing agency, generally as the averaged result of the work of two or more laboratories performing entirely independently. Although the values assigned to company s t a n d a r d s m a y reflect the work of two or more laboratories, absolute assurance t h a t they perform inde pendently is lacking. Therefore company standards can rate no higher t h a n secondary standards and, as such, their use should be limited to internal control analyses. In the case of disagreement be tween producer and consumer with regard to the composition of com mercial items, p r i m a r y s t a n d a r d s m a y be used with much greater con fidence; and the use of company standards in these instances should be only an interim arrangement while awaiting the availability of primary standards. T h e ever-changing character of the p r i m a r y standards needed by industry, plus their diversity a t a n y
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REPORT FOR ANALYTICAL CHEMISTS given time with regard to types, concentration ranges, and amounts required, suggest t h a t a lag between the development of a need a n d its fulfillment is inevitable, Mr. Cooper pointed out. F o r example, x-ray fluorescence methods t h a t became practical about ten years ago imposed special demands with r e gard to dimensions of standard specimens; a n d vacuum optical emission instruments introduced four years ago permitted for t h e first time the determination of certain light elements which now must be provided in spectro-chemical standards. Although t h e internal company standard should a n d does have an important place in our laboratories, p r i m a r y standards evolving from the seasoned judgment a n d object i v i t y of t h e N B S are considered indispensable, M r . Cooper concluded. COMMITTEES
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ANALYTICAL CHEMISTRY
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T h e needs for standard substances are n o t peculiar to the United States, b u t are international in character, D r . Daniel R. Stull of the D o w Chemical Company pointed out. One of t h e international scientific bodies recognizing the need for s t a n d a r d substances is t h e International Union of P u r e and Applied Chemistry ( I U P A C ) , which has a Commission on P h y s ico-chemical S t a n d a r d s a n d D a t a . The members of an I U P A C commission represent their country in the affairs of t h e commission. Itis usual practice in t h e U. S. to have a domestic committee whose function parallels t h a t of t h e I U P A C commission. T h u s , the Committee on Physical Chemistry of t h e N a tional Academy of Sciences—National Research Council ( N A S N R C ) h a s established a Subcommittee on Physico-chemical Standards. T h e Subcommittee on Physicochemical Standards has been active at various times in t h e past, a n d is again becoming active because of the growing need in this area. Efforts are being made to consolidate the national needs for physicochemical standards, and since inter-
national t r a d e requires it, to mesh these national needs with similar international needs. T h e cooperation of academic, industrial, a n d governmental scientists will ensure the formulation of a sound program to meet t h e needs for s t a n d a r d substances, D r . Stull concluded. D r . Stull pointed out t h e need of the chemical industry for a fund of physical properties on t h e chemicals of importance. I n 1955 t h e Manufacturing Chemists' Association ( M C A ) funded a Physical Properties Research Project whose goal w a s t h e preparation of reliable numerical d a t a on chemical materials of importance. This project has recently been made a p a r t of the N a t i o n a l Standard Reference D a t a Program, and experimental measurement of physical properties of chemical materials h a s begun. For these measurements, materials of superior purity are needed, and t h e M C A Physical Properties Proj ect Advisory Subcommittee visualizes t h e need for the establishment of a bank of materials of superior purity. This M C A Subcommittee recently prepared a list of about 100 organic compounds of primary importance. This M C A Priority List of Organic Compounds defines the areas where experimental measurements will first be made, a n d also t h e specific compounds requiring a sample of superior purity. Although the details remain to be worked out, t h e establishment of a sample bank of priority compounds is an important objective of t h e M C A program. ROLE OF A S T M
In a paper presented to t h e Symposium on National a n d I n ternational Standards, J . W. Caum of t h e American Society for Testing and Materials (ASTM) and Harold M. Smith of t h e U. S. Bureau of Mines discussed t h e organization and functions of A S T M . T h e purpose of A S T M is " t h e promotion of knowledge of the materials of engineering a n d the standardization of specifications and t h e methods of testing." T h a t p a r t of A S T M work which has to do with " t h e promotion of knowledge of t h e materials of en-
REPORT
gineering" is effected through in vestigations and researches by com mittees and individual members of the Society and by joint efforts with other groups. The results of these investigations and researches are presented as papers, reports, and discussions at Society and commit tee meetings. Most of them are subsequently published to add to the store of knowledge about the materials of engineering—proper ties, performance under varying or stated conditions, and other infor mation to advance our technology. This is the knowledge on which sound standardization of both specifications and methods of test ing is based. The "standardization of specifi cations and methods of testing" is carried out chiefly by the technical committees of the Society. Each of these committees has under its jurisdiction engineering materials in a definitely prescribed field or some specific phase of testing. Each is a vital and inherent part of the Society.
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THE INTERNATIONAL STANDARDS ORGANIZATION
The work of the International Standards Organization (ISO) is neither known nor understood by a majority of the people of United States industry who really stand to profit most by its efforts. This is the belief of A. C. Webber of E. I. du Pont de Nemours & Co. and Γ. C Frost of the American Standards Association (ASA), expressed in a paper on ISO and ASA given before the Symposium on National and International Standards. The object of ISO is to "promote the development of standardization in the world with a view to facili tating international scientific, tech nological, and economic activity." In effect, this scope permits the consideration of any matters of standardization excepting those concerned with electrical and elec tronic standards which have been the responsibility of the Interna tional Electrotechnical Commission since 1904. The standards bodies of 50 countries are now members of ISO, each participating in those technical committees of interest or economic importance to it.
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REPORT T h e technical work of ISO is car ried out in technical committees. E a c h technical committee is m a d e up of representatives of those mem ber countries which wish to partici pate in its work. There are now 107 technical committees covering a very wide range of subjects. E a c h technical committee has a secretariat, which is responsible for the conduct of the work of the com mittee and for reporting annually to the Council on the results of the year. T h e secretariats are usually accepted on the basis of a major in terest of the member body and ability to p a y the costs of the opera tion. T h e United Kingdom holds 25 secretariats. The United States holds only 10 secretariats and is obviously not carrying a share commensurate with its world trade.
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All technical committees have plenary sessions, some annually and others only when the secretariat feels such a meeting is needed. M a n y of the technical committees have divided the work into specific categories, assigning these to sub committees or working groups un der the leadership and responsibil ity of a separate secretariat. In any case, much of the work m u s t be carried out by correspondence and bv small meetings of interested technical personnel. When a working group of a tech nical committee has completed a draft of nomenclature, method of test, or specifications, it is sub mitted to the member bodies of the technical committee as a D r a f t Proposal. When the ballot of these members shows acceptance b y the majority, the draft, revised if necessary, is submitted to the gen eral secretariat and through it to all 50 member bodies of ISO as a D r a f t ISO Recommendation. Agreement by these members and approval by the Council is then followed bv publication of the mat ter as an ISO Recommendation. I t must be emphasized t h a t these documents are not international standards binding upon the mem ber bodies. T h e y are recommenda tions which are intended to provide a guide to each member bodv for the preparation of its national stnndards. T h e member body in ISO for the United States is the American
REPORT FOR ANALYTICAL CHEMISTS
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I n M r . A d a m s ' opinion, if there Standards Association (ASA). is t o be healthy international trade, ASA was established t o coordinate it must operate within the frame of the standardization efforts of t h e international test methods a n d in major standards-writing bodies in ternational specifications. As more the United States. I t s present and more items move freely in in membership consists of about 140 ternational trade, t h e use of I S O technical societies a n d t r a d e asso test methods and specifications will ciations and 2200 companies. be an automatic development. A When t h e question of American further thought is t h a t t h e agres participation in a n I S O technical sive development and promotion of committee arises, all interested in dustries a n d organizations a r e in ISO test methods and specifications can do much t o stimulate interna formed a n d consulted b y ASA. If tional t r a d e . sufficient interest exists, t h e United States indicates t h a t it wishes t o M a n y factors will affect future participate either actively ( P mem exports from t h e United States, bership) or a s a n observer ( 0 mem some of which m a y be far more bership) in t h e proposed technical i m p o r t a n t t h a n whether or n o t in committee. A committee is then ternational standards are widely organized t o represent t h e United used, M r . A d a m s believes. I S O States in t h e work of t h e technical methods a n d specifications will committee. This committee is a s most certainly be highly effective signed t h e full responsibility for catalytic agents. Standards and the technical work, for t h e estab specifications internationally agreed lishment of t h e American position upon are perhaps the most effective on each item under consideration, aids to overcoming language bar and for t h e provision of delegates riers. Where international stand to meetings. T h e dues t o ISO are ards a n d specifications exist, t h e paid by ASA from its budget, and U. S. commercial position should be staff services a r e provided for t h e the healthiest since materials a n d An automatic pipetting device t h a t r e peatedly delivers accurate, predetermined necessary documentation a n d cor products of submarginal quality quantities of liquid. respondence. I n this manner t h e cannot compete with U. S. quality United States now participates in products. T h e U. S. strength in I M P O R T A N T FEATURES 66 of t h e 107 technical committees, the standards arena stems almost k Hairline "lock-in" micrometer adjust ment for accurate settings * Can b e used holding observer status in t h e r e completely from an industry recog interchangeably with standard lOcc. and maining 41 committees. nition of t h e standardization need Sec. syringes or lcc. tuberculin type syringe and vigorous industry support of To those who a r e familiar with k Newly designed for comfortable grip or the s t a n d a r d s program, M r . Adams the work of I S O a n d who recognize can b e mounted on a laboratory stand k pointed out. its importance, it is clear t h a t t h e All moving parts encased in stainless steel United States participation on t h e I t seems t h a t one of t h e basic * Ideal for washing and diluting proce whole is n o t adequate. While this questions is how far this whole dures where accuracy is important. general low level of participation is standards thing should go, M r . traceable principally t o lack of A d a m s remarked. Certainly if one economic pressures, there is n o t a has a proprietary products—i.e., is sufficient understanding of t h e n a the sole supplier of t h a t product or ture of these international recom material (except in those areas mendations and their potential im where its use m a y have a bearing portance to t h e economic welfare of on the public safety and welfare) — the United States. then t h e standardization m a t t e r is primarily one of quality control b y I n t h e plastics field, t h e interre the company offering t h e product. lationship among t h e American N E W A U P E T T E VALVE — m a d e of durable, However, it is a commercial fact of Chemical Society, A S T M , ASA, i n e r t p l a s t i c —no s p r i n g s —no s e a t e d life t h a t there a r e fewer a n d fewer and I S O has been effective and pro valves, in fact, NO metal and NO moving proprietary products t h a t a r e com parts. Backflow is eliminated and it primes ductive, C. H o w a r d Adams of readily even a t minute settings. T h e pletely controlled b y a single enter Monsanto Chemical C o m p a n y told Aupette Valve is ideal for a variety of prise. I t is M r . A d a m s ' opinion the Symposium on N a t i o n a l and uses in t h e laboratory and is available t h a t supplier a n d consumer will International Standards. One rea separately. operate in a much healthier com son for this m a y be t h a t in m a n y mercial climate if standards defin cases one individual wears t h e Available from your dealer ing product t y p e a n d quality arc necessary number of h a t s t o cover more broadly available, n o t only the various societies a n d organiza domestically, b u t \vorldwide. tions concerned with getting t h e New York 10, Ν. Υ. standards job done. • END
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Circle No. 46 on Readers' Service Card VOL. 36, NO. 12, NOVEMBER 1964
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