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By C. H. Fisher, Abner Eisner

"INTRODUCTION Sulphuric acid of various concentrations has long been used as a reagent in the determination of olefins and aromatics in hydrocarbon oils 4 such as gasoline, kerosene, and neutral oils from coal—tar distillates. Despite its long use, however, there is no general agreement as to optimum conditions and concentration of acid, and numerous methods and modifications have been recommended. In most cases, treatment of the neutral oil with 60 to 90 percent sulphuric acid, followed by distillation to the original endpoint to remove olefin polymers, is recommended for the estimation of unsaturated hydrocarbons. The distillate thus obtained is taken as olefin—free oil and used in later stages of the anlysis. Aromatic hydrocarbons generally are determined in the olefin—free oil by suphonation with more concentrated acid (96 to 100 percent and fuming sulphuric acid are recommended), the hydrocarbons not attacked and removed as water—soluble sulphonic acids being considered as saturated hydrocarbons. In some cases the saturates are examined further by differentiatingbetween cyclic (naphthenes) and acyclic hydrocarbons (paraffins). Generally this is achieved by physical methods, although strong sulphuric acid is known to react preferentially with some types of saturated hydrocarbons,It was the purpose of the present work to make a general study of this type of analysis and to investigate the reactions of hydrocarbons under conditions often used in analyses that employ sulphuric acid reagents. Since previous work is not in good agreement, the optimum concentrations of acid for the different stages of the analysis were determined. Several sulphuric acid methods previously recommended and new modifications were compared, two synthetic solutions being used as the reference oil. The results obtained are presented below under separate headings."

Dec 1, 1937

By C. H. Fisher

Sulphuric acid of various concentrations has long been used as a reagent in the determination of olefins and aromatics in hydrocarbon oils4 such as gasoline, kerosene, and neutral oils from coal-tar distillates. Despite its long use, however, there is no general agreement as to optimum conditions and concentration of acid, and numerous methods and modifications have been recommended. In most cases, treatment of the neutral oil with 80 to 90 percent sulphuric acid, followed by distillation to the original endpoint to remove olefin polymers, is recommended for the estimation of unsaturated hydrocarbons. The distillate thus obtained is taken as olefin-free oil and used in later stages of the anlysis. Aromatic hydrocarbons generally are determined in the olefin-free oil by suphonation with more concentrated acid (96 to 100 percent and fuming sulphuric acid are recommended), the hydrocarbons not attacked and removed as water-soluble sulphoric acids being considered as saturated hydrocarbons. In some cases the saturates are examined further by differentiating between cyclic (naphthenes) and acyclic hydrocarbons (paraffins), Generally this is achieved by physical methods, although strong sulphuric acid is known to react preferentially with some types of saturated hydrocarbons. It was the purpose of the present work to make a general study of this type of analysis and to investigate the reactions of hydrocarbons under conditions often used in analyses that employ sulphuric acid reagents. Since previous work is not in good agreement, the optimum concentrations of acid for the different stages of the analysis were determined. Several sulphuric acid methods previously recommended and new modifications were compared, two synthetic solutions being used as the reference oil. The results obtained are presented below under separate headings.

Jan 1, 1937

By C. H. Fisher

Sulphuric acid of various concentrations has long been used as a reagent in the determination of olefins and aromatics in hydrocarbon oils4 such as gasoline, kerosene, and neutral oils from coal-tar distillates. Despite its long use, however, there is no general agreement as to optimum conditions and concentration of acid, and numerous methods and modifications have been recommended. In most cases, treatment of the neutral oil with 80 to 90 percent sulphuric acid, followed by distillation to the original endpoint to remove olefin polymers, is recommended for the estimation of unsaturated hydrocarbons. The distillate thus obtained is taken as olefin-free oil and used in later stages of the anlysis. Aromatic hydrocarbons generally are determined in the olefin-free oil by suphonation with more concentrated acid (96 to 100 percent and fuming sulphuric acid are recommended), the hydrocarbons not attacked and removed as water-soluble sulphonic acids being considered as saturated hydrocarbons. In some cases the saturates are examined further by differentiating between cyclic (naphthenes) and acyclic hydrocarbons (paraffins), Generally this is achieved by physical methods, although strong sulphuric acid is known to react preferentially with some types of saturated hydrocarbons. It was the purpose of the present work to make a general study of this type of analysis and to investigate the reactions of hydrocarbons under conditions often used in analyses that employ sulphuric acid reagents. Since previous work is not in good agreement, the optimum concentrations of acid for the different stages of the analysis were determined. Several sulphuric acid methods previously recommended and new modifications were compared, two synthetic solutions being used as the reference oil. The results obtained are presented below under separate headings.

Jan 1, 1937

By R. S. Dean

This report, the third of a series of annual reports of the Metallurgical Division to be released in this form, covers the fiscal year July 1, 1936, to June 30, 1937. The technological work of the division is performed by sections. Thus, an efficient organization is provided to prosecute the various problems under investigation, and a logical system is set up for presenting the material contained in this report.

Jan 1, 1937

By R. S. Dean

The work of the metallurgical fundamentals section during the past year, representing active experimental investigation or thermodynamic study, may be summarized as the following problem subjects: 1. Low-temperature specific-heat investigations. 2. Development of a method of concentrating gases. 3. Thermodynamic properties of metallic carbides and nitrides, 4. Production of pure chromium from chromium chlorides. 5. Thermodynamic properties of the hydrates of calcium, sulphate. While this list is not identical, with officially designated problems, due to overlapping of subjects and to new developments within specified problems, presentation upon the basis of this subdivision will best serve to review the work of the section.

Jan 1, 1937

By Walter Murphy

For a number of years the Bureau of Mines has been studying the properties of crude petroleums produced in the United States and the Western Hemisphere. A number of reports have been published giving the analyses of crudes from the different fields and regions as made by the Bureau of Mines Hempel method of analysis.4 Several of these reports include analyses of crude oils from the Rocky Mountain region.5/ The search for new fields and new producing horizons in old fields in the Rocky Mountain region has been quite intensive during the last few years, and a number of discoveries have been made.

Jan 1, 1937

By Walter Murphy

For a number of years the Bureau of Mines has been studying the properties of crude petroleums produced in the United States and the Western Hemisphere. A number of reports have been published giving the analyses of crudes from the different field and regions as made by the Bureau of Mines Hempel method of analysis.4/ Several of these reports include analyses off crude oils from the Rocky Mountain region.5/ The search for new fields and new producing horizons in old fields in the Rocky Mountain region has been quite intensive during the last few years, and a number of discoveries have been made.

Jan 1, 1937

By L. C. IlsLey

The last previous Bureau of Mines publication relative to details of permissible methane detectors (Bulletin 331, published in 1930) describes detectors of four different types, namely flame, combustion, catalytic, and a combination Weatstone-bridge and catalytic type in which catalytic action at the surface of a platinum filament when in methane causes a change in the temperature and resistance of the filament, thus unbalancing the bridge circuit and giving a reading proportional to the methane concentration. Three detractors of the latter type have been approved since 1930. A brief description of each follows: U. C. C. Detector Approval No. 902, covering the U. C. C. indicating detector, as described in Bulletin 331, was extended. January 27, 1930, to cover important changes in design that permit checking the calibration of the detector at any time whether in gas or fresh air. Essential features of the detector are shown in figure 1.

Jan 1, 1937

By L. C. IlsLey

[The last previous Bureau of Mines publication relative to details of permissible methane detectors (Bulletin 331, published in 1930) describes detectors of four different types, namely flame, combustion, catalytic, and a combination Wheatstone-bridge axed catalytic type in which catalytic action at the surface of a platinum filament when in methane causes a change in the temperature and resistance of the filament, thus unbalancing the bridge circuit and giving a reading proportional to the methane concentration. Three detectors of the latter type have been approved since 1933. A brief description of each follows: U. C. C. Detector Approved No. 902, covering the U. C. C. indicating detector, as described in Bulletin 331, was entered January 27, 1330, to cover important chances in design that permit checking; the calibration of the detector at any time, whether in gas or fresh air. Essential features of the detector are shown in figure 1.]

Jan 1, 1937

By J. B. Littlefield

The Greenburg-Smith impinger was developed at the Bureau of Mines in cooperation with the United States Public Health Service in 1922 in the course of an investigation of dust-sampling instruments available at that time. Although it is not used extensively outside of the United States, it is now soused in this country to collect samples for the determination of any dustiness, and most of the information correlating degree of dustiness with physiological effect has been obtained by the impinger method. The chief disadvantages in the use of the regular impinger, especially in mines and other places accessible with difficulty, are its bulk weight, and power requirements. It requires a source either of electricity or of compressed air, which necessitates connections and extension of existing supply lines to each sampling point; the only alternative is the use of a relatively large pump hand-operated with considerable effort.

Jan 1, 1937

By J. B. Littlefield

The Greenburg-Smith impinger was developed at the Bureau of Mines in cooperation with the United States Public Health Service in 1922 in the course of an investigation of dust-sampling instruments available at that time. Although it is not used extensively outside of the United States, it is now soused in this country to collect samples for the determination of any dustiness, and most of the information correlating degree of dustiness with physiological effect has been obtained by the impinger method. The chief disadvantages in the use of the regular impinger, especially in mines and other places accessible with difficulty, are its bulk, weight, and power requirements. It requires a source either of electricity or of compressed air, which necessitates connections and extension of existing supply lines to each sampling point; the only alternative is the use of a relatively large pump hand-operated with considerable effort.

Jan 1, 1937

An active list of permissible explosives was published in December 1936 as part of Bureau of Mines Report of Investigations 3324, under the title "Active List of Permissible Explosives and Blasting Devices Approved Prior to July 31, 1,936." This list included 170 brand names. Changes in the list that have been authorized to June 30, 1937 placed 35 additional brands of permissible explosives on the active permissible list as a result of tests, changes in brand names, or transfer from the inactive list. Ten permissible explosives were transferred from the active to the inactive list. The present list contains 196 brand names, one explosive having been placed on the list subsequent to June 30, 1937. The brand names of the permissible explosives placed on the active list are as follows: [ ]

Jan 1, 1937

An active list of permissible explosives was published in December 1936 as part of Bureau of Mines Report of Investigations 3324, under the title "Active List of Permissible Explosives and Blasting Devices Approved Prior to July 31, 1936." This list included 170 brand names. Changes in the list that have been authorized to June 30, 1937 placed 35 additional brands of permissible explosives on the active permissible list as a result of tests, changes in brand names, or transfer from the inactive list. Ten permissible explosives were transferred from the active to the inactive list. The present list contains 196 brand names, one explosive having been placed on the list subsequent to June 30, 1937. The brand names of the permissible explosives placed on the active list are as follows:

Jan 1, 1937

By E. C. Lane

This paper on the physical and chemical properties of crude oils from California fields is one of a series of reports on the oil-producing districts of the United States. The paper includes a short discussion of results, tabular data, and individual analyses of 16 California crude oils. Analyses of other oil from California have been published in Reports of Investigations 25954/, 26085/, 28466/, and 30747/. The samples were obtained by members of the San Francisco office of the Bureau of Mines. The collecting of the samples vas facilitated by the courtesy of representatives of oil companies in California.

Jan 1, 1937

By E. C. Lane

This paper on the physical and chemical properties of crude oils from California fields is one of a series of reports on the oil-producing districts of the United States. The paper includes a short discussion of results, tabular data, and individual analyses of 16 California crude oils. Analyses of other oil from California have been published in Reports of Investigations 25954/, 26085/ 28466/, and 30747/. The samples were obtained by members of the San Francisco office of the Bureau of Mines. The collecting of the samples vas facilitated by the courtesy of representatives of oil companies in California.

Jan 1, 1937

By L. C. IlsLey

From time to time the Bureau of Mines has issued publications dealing with the various classes of explosion-proof mining machinery that have been tested and approved as permissible for use in mines having atmospheres that may become inflammable by reason of the inadvertent presence of gas or dust. These publications are confined almost entirely to description of the features contributing directly or indirectly to the prevention of explosion or shock hazards, and are intended to give inspectors, safety engineers, and others already familiar with the general safety requirements more detailed information on the safety features of the design of a particular machine. As a background for papers describing permissible machines and to avoid the necessity of duplicating descriptions of methods of conducting investigations and tests of such machinery, Bureau of Mines Bulletin 305, Inspection and Testing of Mine-Type Electrical Equipment for Permissibility, was published in 1929. Three bulletins giving detailed descriptions of the three most numerous types of machines have been issued, viz., Bulletin 313, Permissible Storage-Battery Locomotive and power Trucks. Bulletin 343, Permissible Coal-Handling Equipment. Bulletin 382, Permissible Coal-Cutting Equipment.

Jan 1, 1937

By L. C. IlsLey

From time to time the Bureau of Mines has issued publications dealing with the various classes of explosion-proof mining machinery that have been tested and approved as permissible for use in mines having atmospheres that may become inflammable by reason of the inadvertent presence of gas or dust. These publications are confined almost entirely to description of the features contributing directly or indirectly to the prevention of explosion or shock hazards, and are intended to give inspectors, safety engineers, and others already familiar with the general safety requirements more detailed information on the safety features of the design of a particular machine. As a background for papers describing permissible machines and to avoid the necessity of duplicating descriptions of methods of conducting investigations and tests of such machinery, Bureau of Mines Bulletin 305, Inspection and Testing of Mine-Type Electrical Equipment for Permissibility, was pub¬lished in 1929. Three bulletins giving detailed descriptions of the three most numerous types of machines have been issued, viz., Bulletin 313, Permissible Storage-Battery Locomotive and Power Trucks. Bulletin 343, Permissible Coal-Handling Equipment. Bulletin 392, Permissible Coal-Cutting Equipment.

Jan 1, 1937

By S. R. Zimmerley

[In the course of a flotation investi£ation, a siliceous gold ore was ground in a'ball mill to ':1inns 300-meeh. It wa. found that the small amotIDt of _Ius 300-mesh material had a gole.. assay approximately twice that of the oriGinal ore, &~d that this overs.ize nroduct also contained much abrac..ed iron. .,Joreove I the gold assay of the abraded iron t which was !1epnrated ma§metically', ~iVFl.£ eight ti;nes that of the are. These facts suggested that some r31aticnship ex?...,ted between the abnorma11y high gold content an the prese:1ce of brA-cit)" iron. It was decided, therefore, to investigate furt~er th~ Fl.Gsociation of the bold ~ith the iron abraded from the balls during sri~Qing ]

Jan 1, 1937

By S. R. Zimmerley

[In the course of a flotation investi~ntion, a siliceous gold ore was ground ir, R 'ball mill to ~inils 300-mesh. It mas found that the small mount of zlus 300-~esh mnterial had a go12 assw approximately twice that of the oricinal ors, md thst this oversize ~roduct also contained much abra?.ed iron. >!oreover, the gold assay of the abraded iron, which was separated ma~etic-dl:;, wno ei::ht tiaes tkat of the ore. These facts sug,~estsd th~t sone r3laticnshin existed between the abnormally high .gold content and the preseace of abrade4 iron. It was ciecided, therefore, to investl~ate furtkor ths acsoclation of the ;old nith the iron abraded from the balls durir-g grincing. As a nrelininary ex?rr>hent, a samy?le of siliceous gold ore 786 grolznd for 1-1/2 hours i;l 3 ball mill and the nuln was divided into two products electri~mag-etically. The racult s follow: ]

Jan 1, 1937

By D. J. Parker

On Thursday, March 18, 1937, the country was shocked by news of a terrific explosion at the New London, Tex., school, which caused the death of 280 pupils rind 14 teachers. The explosion occurred at about 3:05 p.m. in the largest of the 11 school buildings on the campus. Figure 1 shows this building, market; "Main high school building?, with respect to other buildings, pipe lines, oil wells, and gas lines on the property.

Jan 1, 1937