The usual procedure for the preparation of carbon dioxide from the oxalic-acid standard supplied by the National Bureau of Standards is wet oxidation by means of potassium permanganate in acid solution. The procedure is straightforward, but suffers from a certain difficulty in determining the end point of the reaction.

The present list comprises only research projects undertaken by the laboratory on the validity of radiocarbon dating of soil, shell, coral and very old samples, all in presence of suspected contamination. All measurements were performed on a Beckman LS-200 liquid scintillation spectrometer (Radiocarbon, 1968, v. 10, p. 179-199). The chemical treatment of samples is given within the text of each section.

Measurements have continued with the 6 L counter. A counter of similar design but with 1 L volume has recently been brought into operation. Despite replacement of the teflon parts, the 1.5 L Oeschger-type counter has not worked consistently and has not been used for dating. Results are not corrected for δ C13. Errors quoted refer only to the standard deviation calculated from a statistical analysis of count rates and the Libby half-life of 5570 ± 30 yr.

Alkali pretreatment is used for all samples of charcoal, peat, wood, and plant material provided they are of sufficient quantity. It is now standard practice to boil the sample in 5% HCl solution and filter, both before and after boiling it in 2% NaOH solution. Between each treatment it is washed in boiling distilled water and is finally oven dried at 110°C. Concentrations of acid and alkalis are varied to suit each sample but the sequence of the pretreatment is always the same. In some cases a humate extract is obtained by precipitation with weak acid from the alkali solution filtrate.

The collagen fraction is obtained from samples of bone using the method of Krueger (1966) by treatment with dilute acid under reduced pressure. The gas evolved during the treatment is usually discarded but is occasionally retained and dated as the mineral fraction.

After mechanical cleaning, samples of shell are dissolved in stages with 6N HCl to divide them into two or three fractions corresponding to the outer, middle, and inner layers of the shell. Normally the outer fraction is discarded when three fractions have been prepared.

This list includes most of the dates produced from September 1967 to April 1968. The laboratory continues to use the benzene method of the previous date list (Radiocarbon, 1968, v. 10, p. 8–28); however, the counter and chemical treatment equipment were transferred to a field laboratory in order to avoid any possibility of contamination. Two new benzene synthesis lines of our own construction were added to the commercial unit. Their operation is excellent and over-all costs were nominal.

The following list includes selected geologic and pollen dated samples measured since 1965. After moving to new laboratory quarters, we increased shielding to 470 g/cm2 on all sides and 660g/cm2 at the top. Background of our Houtermans-Oeschger-type counters filled with 700 mm Hg of acetylene is now:

Age calculations in this list include samples dated since January, 1967. Samples are converted to benzene and counted in a liquid scintillation spectrometer. Operations are essentially the same as those described in Radiocarbon, 1966, v. 8, p. 46–53 and Radiocarbon, 1967, v. 9, p. 38–42. Modern reference is 95% the activity of NBS oxalic acid standard, not age-corrected wood as reported in Radiocarbon, 1966, v. 8, p. 46–53.

Dates listed below are based on measurements made up to May 1968, and cover a period during which the technique of gas proportional counting using CO2 was gradually replaced by liquid scintillation counting using benzene. The gas counting measurements were carried out by the method and techniques previously described (Barker and Mackey, 1968) the only modifications being the replacement of some old electronic units by more stable solid-state equipment; proportional counting results are indicated in the text by (P) at the end of the relevant sample descriptions. Liquid scintillation counting, which is now the preferred method in this laboratory, is carried out using a Packard Tri-Carb liquid scintillation spectrometer model 3315/AES fitted with selected low-noise quartz-faced photomultipliers. Normally 3 ml of benzene is prepared from each sample. This is dissolved in 12 ml of scintillation grade toluene containing 5 gm/liter of scintillator (PPO) and the solution is measured in a standard low-potassium glass vial at a temperature of 0°C. Photomultiplier E.H.T., amplifier, and channel width settings are optimized for C14, and measurements are carried out at ca. 65% efficiency of detection for C14 to eliminate interference from any tritium which may be present in the benzene. Under these circumstances the background is approx. 8.6 cpm and the modern (95% Aox) is approx. 24.0 cpm. Samples are counted in groups of 3 to 5 together with background and modern reference samples and are measured for at least one week, the instrument being set to cycle at 100 min intervals. In this period, the counts accumulated are such that the background is always measured to a statistical accuracy of better than 1% and most other samples to a higher accuracy than this. Background and modern counts used in the calculation of each result are only those relevant to the period of measurement of that particular sample. Statistical analysis of groups of replicate measurements made under these conditions over a very long period of time has demonstrated the excellent long-term stability of the equipment and indicates that the technique is quite capable of achieving results of very high statistical accuracy when required.

The Radiocarbon Dating Laboratory of the Geological Survey of Canada routinely operates two proportional counters; one 2 L and one 5 L. The 2 L counter is operated entirely at 2 atm. and the 5 L counter mainly at 1 atm. On occasion the 5 L counter is operated at 4 atm. Detailed descriptions of these two counters have recently been published (Dyck, 1967a). A I L counter has been fabricated and is now undergoing preliminary testing.

Two radiocarbon counting systems have been established in the Chemistry Department, University of Glasgow, since late 1967.

The counting gas is methane, at pressures up to 10 atm, and 2 alternative procedures are followed for methane production, (a) high pressure synthesis in a stainless steel 4.5 1 reactor and (b) low pressure synthesis in an all glass flow-reactor. Both systems employ 0.5% ruthenium on alumina pellets as catalyst (Engelhard Industries Ltd.). Early samples synthesized with Air Products' hydrogen showed evidence of tritium contamination. This gas supply was later replaced with tritium-free hydrogen supplied by Messrs. Griesheim, Düsseldorf, Germany. Both detectors used for routine measurements are 0.5 1 internal gas counters supplied by Beckman Instruments Inc., California. The detectors are surrounded by a concentric-wall multiple anode anticoincidence counter. The entire counter assembly is encased within a 4-in.-thick lead shield manufactured from aged lead by J. Girdler and Co., London. Counter electronics, anticoincidence system and power supply are of Beckman design (Sharp and Ellis, 1965).

This list continues Gakushuin VI (Radiocarbon, 1967, v. 9, p. 43-62), the same instruments and techniques having been employed.

Age calculations are based on the Libby half-life of C14, 5570 ± 30 years, and the modern activity given by 0.95 Aox, i.e., 95% of the activity of NBS oxalic acid standard. The errors quoted are the standard deviation obtained from the number of counts only. When observed activity is less than 2σ above background, infinite date is given with a limit corresponding to the activity of 3σ, and when it is greater than 0.95 Aox −2σ, modern date is given with a limit = 0.95 Aox —3σ. For shell samples, dates are computed without any correction for environmental and biological isotopic fractionation.

The description and comments are essentially those of the submitters.

The dates detailed below are a selection of C14 dates obtained from February 1966 to December 1967 for geologic samples. The method is essentially the same as described previously in Radiocarbon, 1966, v. 8 p. 74-95. All samples were subjected to pretreatment, differing in individual cases, to remove contamination. On one of our three installations, modern transistorized equipment replaced the original electronics.

All dates reported have been calculated on the assumed half-life of 5568 yr for C14, and of 1950 as the reference year.

The following list presents dates on a portion of the samples measured at ISOTOPES during 1967 and 1968 and measurements made previously for which either complete sample data has been recently received, or, in some cases, deferred due to the editorial load in preparing the definitive list.

This list reports certain measurements made from 1965 to 1967. These samples are devoted to a special study of organic matter in soils. The work in large part is the subject of a thesis defended in Paris by S. M. Nakhla, 1968.

The following list comprises selected measurements made during 1967–68. The method is essentially the same as previously described. A 0.6 L proportional gas-counter at 3 atm CH4 pressure is used. Ages are given relative to A.D. 1950 and half-life of 5570 yr has been assumed. The quoted error is the experimental standard deviation and includes the uncertainty on the unknown sample, the modern standard and the background.

The Radiocarbon Dating Laboratory was founded in 1965 by the Department of Geology, University of Lyon, to study the Late Quaternary geology of the Rhone-Alps Region, and to contribute to hydrogeologic and archaeologic studies. It has been installed in the basement of the Nuclear Physics Institute. Preparation began in 1966 and first dates obtained in June 1967.

This list contains dates for Latin America which have mainly been measured during the past few years. The results are grouped into three categories: geologic, archaeologic, and geophysical, and arranged according to the country of provenance, passing roughly from N to S. Most of the geologic samples are connected with palynologic studies. In cases where the influence of man is apparent in the pollen diagrams, this is explicitly mentioned. Descriptions and comments are based on information provided by the collectors or submitters and on the publications referred to under each sample or series. For the archaeologic section reference has also been made to the general works of Meggers and Evans (1963), Jennings and Norbeck (1964), and Willey (1966).

The following list of dates contains most of the measurements obtained since our last list. Procedures of measurements and calculation are as previously described in Radiocarbon, 1964, v. 6, p. 194–196; 1966, v. 8, p. 286–291. A new 1.1 L counter, all metal and quartz, built in the laboratory has been in use since 1967.

This study was started during the summer of 1965 because of the discrepancy observed between dates obtained from wood charcoal and charred corn samples collected from the same archaeologic sites. These results are listed in Table 1.

The following list comprises measurements made since those reported in NPL V.

No changes have been made in measurement technique or in the method of calculating results described in NPL III.

The radiocarbon dating laboratory of the Illinois State Geological Survey has been established to satisfy a growing need for radiocarbon dates for an active Pleistocene research program. Because of the age and type of material dated, the benzene liquid scintillation counting method is employed in this laboratory. The detailed chemical procedure for converting carbon to benzene has been published by Noakes, Kim, and Stipp (1965) and Noakes, Kim, and Akers (1967); however, the procedures for benzene synthesis and sample counting are briefly explained below to clarify this laboratory's procedure.

An organic sample, such as peat, organic silt, or wood, is burned and the CO2 evolved is absorbed in NH4OH. SrCl2 solution is added to precipitate the carbonate, and the solution plus precipitate is boiled and cooled before filtration of SrCO3. The SrCO3 is acidified with dilute H3PO4 to liberate CO2 in a closed system, and the CO2 is converted to C2H2, as reported by Barker (1953). In this method, 2.4 gm of dry packed lithium, obtainable from the Lithium Corporation of America, is used for each liter of CO2 that is converted to C2H2. Trimerization of the C2H2 to form C6H6 is accomplished using a vanadium-alumina catalyst.

To the C6H6 synthesized from the sample carbon, 2 cc of toluene containing 100 mg Butyl-PBD, 2-(4-tert-Butylphenyl)-5-(4-Biphenylyl)-1,3,4-Oxadiazole, are added, and this mixture is made to a total volume of 10 cc with spectrograde C6H6. A modified Packard Instrument Co. liquid scintillation spectrometer (Model 3375) is used for measurement of C14 activity.

Ages are calculated from a C14 half-life of 5568 years, and the standard deviation (1σ) is based only on counting errors; however, if calculated error is less than 200 years, 200 years is chosen as one standard deviation (1σ).