Direct standard calibration

In the direct standard calibration method, narrowly distributed standards of the same polymer being analyzed are used. The retention volume at the peak maximum of each standard is equated with its stated molecular weight. This is the simplest method, but it is generally restricted in its utility owing to the lack of availability of many different polymer standard types. It also requires a sufficient number of standards of different molecular weights to cover completely the entire dynamic range of the column set or, at least, the range of molecular... 

In the direct standardization introduced by Wang et al. [42] one finds the transformation needed to transfer spectra from the child instrument to the parent instrument using a multivariate calibration model for the transformation matrix = ZgF. The transformation matrix F (qxq) translates spectra Zg that are actually measured on the child instrument B into spectra Z that appear as if they were measured on instrument A. Predictions are then obtained by applying the old calibration model to these simulated spectra Z ... 

Now, it is necessary to calibrate the calorimeter in order to analyze quantitatively the recorded thermograms and determine the amount of heat evolved by the interaction of a dose of gas with the adsorbent surface. The use of a standard substance or of a standard reaction is certainly the most simple and reliable method, though indirect, for calibrating a calorimeter, since it does not require any modification of the inner cell arrangement. [For a recent review on calibration procedures, see 72).3 No standard adsorbent-adsorbate system has been defined, however, and the direct electrical calibration must therefore be used. It should be remarked, moreover, that the comparison of the experimental heat of a catalytic reaction with the known change of enthalpy associated with the reaction at the same temperature provides, in some favorable cases, a direct control of the electrical calibration (see Section VII.C). 

The pH meter is standardized (calibrated) with the use of buffer solutions. Usually, two buffer solutions are used for maximum accuracy. The pH values for these solutions should bracket the pH value expected for the sample. For example, if the pH of a sample to be measured is expected to be 9.0, buffers of pH = 7.0 and pH = 10.0 should be used. Buffers with pH values of 4.0,7.0, and 10.0 are available commercially specifically for pH meter standardization. Alternatively, of course, homemade buffer solutions (see Chapter 5) may be used. In either case, when the pH electrode and reference electrode are immersed in the buffer solution being measured and the electrode leads are connected to the pH meter, the meter reading is electronically adjusted (refer to manufacturer s literature for specifics) to read the pH of this soluiton. The electrodes can then be immersed into the solution being tested and the pH directly determined. 

Procedure A standard calibration curve is plotted by thoroughly mixing together about 10% (w/w) of the analyte with the KBr-KSCN mixture and then grinding the same intimately. Now, the ratio of the thiocyanate absorption at 2125 cm-1 to a selected band absorption of the analyte is plotted against the percent concentration of the sample. Likewise, an identical disc is prepared with the unknown sample and the same KBr-KSCN mixture. Finally, its absorbance ratio is determined and the concentration (of unknown sample) is read off directly from the standard calibration curve. 

Standardizing the spectral response is mathematically more complex than standardizing the calibration models but provides better results as it allows slight spectral differences - the most common between very similar instruments - to be corrected via simple calculations. More marked differences can be accommodated with more complex and specific algorithms. This approach compares spectra recorded on different instruments, which are used to derive a mathematical equation, allowing their spectral response to be mutually correlated. The equation is then used to correct the new spectra recorded on the slave, which are thus made more similar to those obtained with the master. The simplest methods used in this context are of the univariate type, which correlate each wavelength in two spectra in a direct, simple manner. These methods, however, are only effective with very simple spectral differences. On the other hand, multivariate methods allow the construction of matrices correlating bodies of spectra recorded on different instruments for the above-described purpose. The most frequent choice in this context is piecewise direct standardization... 

Calibration Calibration entails the adjustment of a measurement device so that the value from the measurement device agrees with the value from a standard. The International Standards Organization (ISO) has developed a number of standards specifically directed to calibration of measurement devices. Furthermore, compliance with the ISO 9000 standards requires that the working standard used to calibrate a measurement device be traceable to an internationally recognized standard such as those maintained by the National Institute of Standards and Technology (NIST). 

ID MS involves the precise addition of an isotopically labeled form of the analyte to an accurately measured sample of the specimen, e.g., serum. After an appropriate equilibration time, the analyte and its labeled internal standard are isolated from the sample with a suitable extraction and purification step, and an aliquot is introduced, either directly or after (gas) chromatographic separation from remaining interferences, into the mass spectrometer. The latter accurately measures the ratio of analyte to internal standard using the intensities of an equivalent ion in the spectrum of each. From this ratio, the concentration of analyte is calculated by comparison with the ratios of the same ions in standard calibration mixtures. Critical points in this procedure are as follows ... 

The goal of methods that standardize instrument response is to find a function that maps the response of the secondary instrument to match the response of the primary instrument. This concept is used in the statistical analysis procedure known as Procrustes analysis [97], One such method for standardizing instrument response is the piecewise direct standardization (PDS) method, first described in 1991 [98,100], PDS was designed to compensate for mismatches between spectroscopic instruments due to small differences in optical alignment, gratings, light sources, detectors, etc. The method has been demonstrated to work well in many NIR assays where PCR or PLS calibration models are used with a small number of factors. 

System Suitability Chromatograph a suitable number of injections of 1 mg each of USP Alpha Tocopherol Reference Standard and USP Alpha Tocopheryl Acetate Reference Standard per milliliter of w-hcxanc, as directed under Calibration (below), to ensure that the resolution factor, R, is not less than 1.0 (see System Suitability in High-Performance Liquid Chromatography under Chromatography, Appendix HA). 

Calibration is carried out using standard calibration curves. The simplicity, repeatability, and low cost of the method have allowed its use for routine determination of trihalomethanes in tap water. SOME has also been compared with solid phase microextraction (SPME), purge and trap (P T), and direct aqueous injection (DAI) [10]. This technique offers accuracy comparable with that obtained using P T and DAI. With respect to conventional LEE, the SDME method is more accurate. In contrast to DAI and P T, it requires no special equipment. SDME has been used for extraction of chlorophenols [II], pesticides [12, 13], warfare agents [14], and butanone derivatives [15], and for control of food products [16]. The low costs of the SDME method (typical GC syringe and 2-3 pL of solvent), simplicity, and short extraction time (approximately 15 min) make it particularly suitable for preliminary analyses of organic pollutants in water samples. It can also be an effective alternative to SPME, as it does not require the use of expensive instrumentation. 

Direct column calibration for a given polymer requires the use of narrow MWD samples of that polymer, with molecular weights covering the whole range of interest. The polydispersity of the calibration standards must be less than 1.05, except for the very low and very high MWs (< 10 and > 10 ), for which polydispersity can reach 1.20. The chromatograms of such standards give narrow peaks and to each standard is associated the retention volume of the peak maximum. 

The experimental dependence M = /(V), i.e. the classical SEC calibration curve usually obtained by using narrow standards, in such a case can be obtained directly without calibration from the on-line LS detector. By combining the experimental function M = /(V) and the concentration profile (from DRI), one can construct the complete MMD of the HA sample. The differential and cumulative MMD of a high molar mass HA sample (Mw = 652 kDa, D = 2.1) are shown in Fig. (10). Starting from the initial MMD, the molecular weight averages and dispersity index (Mn, Mw, Mz, and D) could be easily calculated using the appropriate definitions. 

Internal standard External standard Calibration method Number of calibration standards Finear range of calibration direct/standard additions... 

Internal standard calibration similarly requires the preparation of external standard solutions, but in addition a constant concentration of a second compound is added to each sample. The sample concentration is directly proportional to the ratio of the analyte to internal standard. This method is used for the analysis of biological samples and other more difficult analyses. 

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