Journal of Research of the National Institute of Standards and Technology最新文献

Between 1911 and 1984, the National Bureau of Standards (NBS) conducted a large number of corrosion studies that included the measurement of corrosion damage to samples exposed to real-world environments. One of these studies was an investigation conducted between 1922 and 1940 into the corrosion of bare steel and wrought iron pipes buried underground at 47 different sites representing different soil types across the Unites States. At the start of this study, very little was known about the corrosion of ferrous alloys underground. The objectives of this study were to determine (i) if coatings would be required to prevent corrosion, and (ii) if soil properties could be used to predict corrosion and determine when coatings would be required. While this study determined very quickly that coatings would be required for some soils, it found that the results were so divergent that even generalities based on this data must be drawn with care. The investigators concluded that so many diverse factors influence corrosion rates underground that planning of proper tests and interpretation of the results were matters of considerable difficulty and that quantitative interpretations or extrapolations could be done "only in approximate fashion" and attempted only in the "restricted area" of the tests until more complete information is available. Following the passage of the Pipeline Safety Improvement Act in 2002 and at the urging of the pipeline industry, the Office of Pipeline Safety of the U.S. Department of Transportation approached the National Institute of Standards and Technology (NBS became NIST in 1988) and requested that the data from this study be reexamined to determine if the information handling and analysis capabilities of modern computers and software could enable the extraction of more meaningful information from these data. This report is a summary of the resulting investigations. The data from the original NBS studies were analyzed using a variety of commercially available software packages for statistical analysis. The emphasis was on identifying trends in the data that could be later exploited in the development of an empirical model for predicting the range of expected corrosion behavior for any given set of soil chemistry and conditions. A large number of issues were identified with this corrosion dataset, but given the limited knowledge of corrosion and statistical analysis at the time the study was conducted, these shortcomings are not surprising and many of these were recognized by the investigators before the study was concluded. However, it is important to keep in mind that complete soil data is provided for less than half of the sites in this study. In agreement with the initial study, it was concluded that any differences in the corrosion behavior of the alloys could not be resolved due to the scatter in the results from the environmental factors and no significant difference could be determined between alloys. Linear regressi

We describe a method to estimate the scale errors in the horizontal angle encoder of a laser tracker in this paper. The method does not require expensive instrumentation such as a rotary stage or even a calibrated artifact. An uncalibrated but stable length is realized between two targets mounted on stands that are at tracker height. The tracker measures the distance between these two targets from different azimuthal positions (say, in intervals of 20° over 360°). Each target is measured in both front face and back face. Low order harmonic scale errors can be estimated from this data and may then be used to correct the encoder's error map to improve the tracker's angle measurement accuracy. We have demonstrated this for the second order harmonic in this paper. It is important to compensate for even order harmonics as their influence cannot be removed by averaging front face and back face measurements whereas odd orders can be removed by averaging. We tested six trackers from three different manufacturers. Two of those trackers are newer models introduced at the time of writing of this paper. For older trackers from two manufacturers, the length errors in a 7.75 m horizontal length placed 7 m away from a tracker were of the order of ± 65 μm before correcting the error map. They reduced to less than ± 25 μm after correcting the error map for second order scale errors. Newer trackers from the same manufacturers did not show this error. An older tracker from a third manufacturer also did not show this error.

Veneering ceramics designed to be used with modern zirconia framework restorations have been reported to fracture occasionally in vivo. The fracture toughness of such veneering ceramics was measured and compared to that of conventional feldspathic porcelain veneering ceramics for metal framework restorations. The fracture toughness of the leucite free veneer was measured to be 0.73 MPa m ± 0.02 MPa m, which is less than that for the porcelain fused to metal (PFM) veneering ceramic: 1.10 MPa ± 0.2 MPa. (Uncertainties are one standard deviation unless otherwise noted.) The surface crack in flexure (SCF) method was suitable for both materials, but precrack identification was difficult for the leucite containing feldspathic porcelain PFM veneer.

Previous studies reported premixed calcium phosphate cements (CPCs) that were stable in the package and form hydroxyapatite (HA) as the product after exposure to an aqueous environment. These cements had setting times of greater than 60 min, which are too long to be useful for some clinical applications. The present study investigated properties of fast-setting HA-forming premixed CPCs that initially consisted of two separate premixed pastes: (1) finely ground (1.0 μm in median size) dicalcium phosphate anhydrous (DCPA) mixed with an aqueous NaH(2)PO(4) solution, 1.5 mol/L or 3.0 mol/L in concentration, and (2) tetracalcium phosphate consisting of combinations of particles of two different size distributions, 5 μm (TTCP5) and 17 μm (TTCP17) in median size, mixed with glycerin. Equal volume of Pastes 1 and 2 were injected with the use of atwo-barrel syringe fitted with a static mixer into sample molds. The molar Ca/P ratio of combined paste was approximately 1.5. Cements were characterized in terms of setting time (Gilmore needle), diametral tensile strength (DTS), and phase composition (powder x-ray diffraction, XRD). Setting times were found to range from (4.3 ± 0.6 to 68 ± 3) min (mean ± sd; n = 3), and 1-d and 7-d DTS values were from (0.89 ± 0.08 to 2.44 ± 0.16) MPa (mean ± sd; n = 5). Both the NaH(2)PO(4) concentration and TTCP particle size distribution had significant (p < 0.01) effects on setting time and DTS. Powder XRD analysis showed that low crystallinity HA and unreacted DCPA were present in the 1-day specimens, and the extent of HA formation increased with increasing amount of TTCP5 in the TTCP paste. CONCLUSION: Injectable HA-forming premixed CPCs with setting times from 4 to 70 min can be prepared by using DCPA and TTCP as the ingredients. Compared to the conventional powder liquid cements, these premixed CPCs have the advantages of being easy to use and having a range of hardening times.

This study reports for the first time in vitro and in vivo properties of fluorapatite (FA)-forming calcium phosphate cements (CPCs). The experimental cements contained from (0 to 3.1) mass % of F, corresponding to presence of FA at levels of approximately (0 to 87) mass %. The crystallinity of the apatitic cement product increased greatly with the FA content. When implanted subcutaneously in rats, the in vivo resorption rate decreased significantly with increasing FA content. The cement with the highest FA content was not resorbed in soft tissue, making it the first known biocompatible and bioinert CPC. These bioinert CPCs might be useful for applications where slow or no resorption of the implant is required to achieve the desired clinical outcome.

Diffusion-controlled dissolution and precipitation reactions occur in many biological systems and some non-stirred in vitro systems. Previous studies have shown that differences in the diffusion rates of the ions involved in a dissolution/precipitation reaction can produce significant effects on the rate and course of the reaction. We report here results of a study that show inter-diffusion of ions between two solutions, both saturated with respect to hydroxyapatite but with dissimilar compositions, resulted in one solution becoming undersaturated and the other supersaturated. A model is proposed that may explain the formation of a mineral-dense layer in the caries process.

The bone defect repair functions of calcium phosphate cement (CPC) are related to its osteoconductivity and its gradual replacement by new bone. Adding mannitol to CPC may enhance its bone repair potential by increasing CPCs macroporosity and dissolution rate. The objective of the study was to assess microporosity and macroporosity and dissolution rates for CPC mixed with mannitol. Three groups of CPC discs were prepared by combining an equimolar mixture of tetracalcium phosphate and anhydrous dicalcium phosphate with (0 %, 10 %, or 50 %) mass fraction (hereafter expressed as mass %) of mannitol. Macroporosity and microporosity of the samples were calculated from volume and mass measurements of the discs. Discs were then placed in a pH 3.0 demineralizing solution simulating acidified physiological solution, and dissolution rates were measured by a previously described constant-composition titration method. Pure CPC exhibited no macropores and microporosity (mean ± s.d.; n = 5) of (46.8 ± 0.8) % volume fraction (hereafter expressed as vol %). Adding 10 mass % mannitol resulted in 15.6 ± 3.9 vol % macroporosity and 39.4 ± 1.8 vol % microporosity, and adding 50 mass % mannitol produced 54.7 ± 0.8 vol % macroporosity and 21.1 ± 0.4 vol % microporosity. The dissolution rates (mean ± s.d.; n = 5) of CPC with (0, 10, and 50) mass % mannitol incorporation were (30.6 ± 3.4, 44.8 ± 10.2, and 54.7 ± 3.6, respectively) μg · cm(-2) · min(-1), or (0.018 ± 0.002, 0.032 ± 0.007, and 0.072 ± 0.005, respectively) μL · cm(-2) · min(-1). Adding either 10 mass % or 50 mass % mannitol into CPC significantly (p < 0.05) increased CPC dissolution rates. Adding mannitol readily increased macroporosity and dissolution rate of CPC, which may enhance the capacity of CPC to be osteoconductive.

Previous studies showed that water-free, premixed calcium phosphate cements (Pre-CPCs) exhibited longer hardening times and lower strengths than conventional CPCs, but were stable in the package. The materials hardened only after being delivered to a wet environment and formed hydroxyapatite as the only product. Pre-CPCs also demonstrated good washout resistance and excellent biocompatibility when implanted in subcutaneous tissues in rats. The present study evaluated characteristics of Pre-CPCs when implanted in subcutaneous tissues (Study I) and used for repairing surgically created two-wall periodontal defects (Study II). Pre-CPC pastes were prepared by combining CPC powders that consisted of CPC-1: Ca(4)(PO(4))(2)O and CaHPO(4), CPC-2: α-Ca(3)(PO(4))(2) and CaCO(3) or CPC-3: DCPA and Ca(OH)(2) with a glycerol at powder-to-liquid mass ratios of 3.5, 2.5, and 2.5, respectively. In each cement mixture, the Ca to P molar ratio was 1.67. The glycerol contained Na(2)HPO(4) (30 mass %) and hydroxypropyl methylcellulose (0.55 %) to accelerate cement hardening and improve washout resistance, respectively. In Study I, the test materials were implanted subcutaneously in rats. Four weeks after the operation, the animals were sacrificed and histopathological observations were performed. The results showed that all of the implanted materials exhibited very slight or negligible inflammatory reactions in tissues contacted with the implants. In Study II, the mandibular premolar teeth of mature beagle dogs were extracted. One month later, two-wall periodontal bone defects were surgically created adjacent to the teeth of the mandibular bone. The defects were filled with the Pre-CPC pastes and the flaps replaced in the preoperative position. The dogs were sacrificed at 1, 3 and 6 months after surgery and sections of filled defects resected. Results showed that one month after surgery, the implanted Pre-CPC-1 paste was partially replaced by bone and was converted to bone at 6 months. The pockets filled with Pre-CPC-2 were completely covered by newly formed bone in 1 month. The Pre-CPC-2 was partially replaced by trabecular bone in 1 month and was completely replaced by bone in 6 months. Examination of 1 month and 3 month samples indicated that Pre-CPC-2 resorbed and was replaced by bone more rapidly than Pre-CPC 1. Both Pre-CPC pastes were highly osteoconductive. When implanted in periodontal defects, Pre-CPC-2 was replaced by bone more rapidly than Pre-CPC-1.

This study aimed at preparing and studying the properties of nanoparticles of calcium phosphate (nCaP) with Ca/P ratios ranging from 1.0 to 1.67 using a spray-drying technique. Micro-structural analyses suggested that the nCaPs with Ca/P ratios of 1.67 to 1.33 were nano-sized amorphous calcium phosphate (ACP) containing varying amounts of acid phosphate and carbonate. The nCaP with Ca/P ratio of 1 contained only nano-sized low crystalline dicalcium phosphate (DCP). BET measurements of the nCaPs showed specific surface areas of (12 ± 2 to 50 ± 1) m(2)/g, corresponding to estimated equivalent spherical diameters of (38 to 172) nm. However, dynamic light scattering measurements revealed much larger particles of (380 ± 49 to 768 ± 111) nm, owing to agglomeration of the smaller primary nano particles as revealed by Scanning Electron Microscopy (SEM). Thermodynamic solubility measurements showed that the nCaPs with Ca/P ratio of 1.33 - 1.67 all have similar solubility behavior. The materials were more soluble than the crystalline hydroxyapatite (HA) at pH greater than about 4.7, and more soluble than β-tricalcium phosphate (β-TCP), octacalcium phosphate (OCP) and DCP at pH above 5.5. Their solubility approached that of α-tricalcium phosphate (α-TCP) at about pH 7. These nCaPs, which cannot be readily prepared by other currently available methods for nanoparticle preparation, have potential biomedical applications.