Repeatability weighing

Repeatability Obtain as standard deviation of repeated weighings or assume part of repeatability of measurement = s. = 0.2 mg... 

In the Poisson and binomial distributions, the mean and variance are not independent quantities, and in the Poisson distribution they are equal. This is not an appropriate description of most measurements or observations, where the variance depends on the type of experiment. For example, a series of repeated weighings of an object will give an average value, but the spread of the observed values will depend on the quality and precision of the balance used. In other words, the mean and variance are independent quantities, and different two parameter statistical distribution functions are needed to describe these situations. The most celebrated such function is the Gaussian, or normal, distribution ... 

At some level of measurement there may be some variation in repeated weighings but we expect this to be extremely small compared with the weight itself - so the balance weighs with good precision as well as good accuracy. 

Depending on the analytical requirements, samples may be stabilised in readiness for further preparation by freezing, freeze drying, air drying or oven drying at low temperature (typically 30-35°C) until the sample weight is approximately constant (i.e. a within 5% variation on repeated weighings). 

Repeatability of weighings M(baliprec) SD from 10 repeated weighings of 10 mg standard mass = 0.024 mg 0.024 mg —... 

Repeated weighing until an equilibrium weight is attained... 

Scientists often repeat measurements several times to increase confidence in the result. We can distinguish between two different kinds of certainty—called accuracy and precision—associated with such measurements. Accuracy refers to how close the measured value is to the actual value. Precision refers to how close a series of measurements are to one another or how reproducible they are. A series of measurements can be precise (close to one another in value and reproducible) but not accurate (not close to the true value). Consider the results of three students who repeatedly weighed a lead block known to have a true mass of 10.00 g (indicated by the solid horizontal blue line on the graphs). 

Alternately, obtain the sample injection device mass before and after injection to determine the amount of sample injected. This method provides greater predsion than the volume delivery method, provided a balance w th a precision of 0.01 mg is used and the syringe is carefully handled to obtain repeatable weighings. 

Then again remove T, and drop a weighed pellet of the solute through the side arm A. Stir the mixture until a clear solution is obtained, and then repeat the above process until three consistent readings of the freezing point of the solution have been obtained. Then add a second weighed pellet of the solute, and determine the freezing-p>oint of this more concentrated solution in the same way. 

Wait a few minutes after the pellet has completely dissolved, and then continue taking readings as before until three consistent values are obtained. A second weighed pellet may then be added if desired, and the process repeated. 

Weigh out accurately about 2 g. of glycine, transfer to a 250 ml. graduated flask, dissolve in distilled water, make up to the mark, and mix well. Transfer 25 ml. of the solution to a conical flask, add 2 drops of phenolphthalein, and then again add dilute sodium hydroxide very carefully until the solution is just faintly pink. No v add about 10 ml. (/. ., an excess) of the neutralised formaldehyde solution the pink colour of the phenolphthalein disappears immediately and the solution becomes markedly acid. Titrate with AI io sodium hydroxide solution until the pink colour is just restored. Repeat the process with at least two further quantities of 25 ml. of the glycine solution in order to obtain consistent readings. 

The whole process is then repeated exactly as described above. The absorption tubes are then weighed and attached to the apparatus ffull details will be given below when a complete combustion is described), and the above process repeated. The absorption tubes are detached and reweighed. They should not have gained in weight by more than o i... 

It is instructive for the student to construct a rough melting point diagram (compare Section 1,13 and Fig. 1,12, 1) for mixtures of cinnamic acid and urea. Weigh out 1 00 g. each of the two finely powdered components, and divide each into ten approximately equal portions on a sheet of clean, smooth paper. Mix 4 portions of cinnamic acid (A) with 1 portion of urea B) intimately with the aid of a spatula on a glass slide, and determine the melting point (the temperature at which the mixture just becomes completely fluid is noted). Repeat the procedure for 3 parts of A and 2 parts oiB 2 parts of A and 3 parts of B and 1 part of A and 4 parts of B. Tabulate your results as follows —... 

A solution of 66.5 g. (1.01 moles) of 85% potassium hydroxide in 300 ml. of water in an 800-ml. beaker is heated to 60-70 , and 100 g. (0.505 mole) of commercial 1,8-naphthalic anhydride (Note 1) is stirred in. The pH of the resultant deep-brown solution is adjusted to a value of 7 (Note 2) with 6N hydrochloric acid and 3N potassium hydroxide. It is treated with 10 g. of decolorizing carbon and filtered. This operation is repeated. The filtrate is concentrated in a 1.5-1. beaker on a steam bath to about 180 ml. The concentrate is cooled to room temperature, 800 ml. of methanol is added with vigorous stirring by hand, and the mixture is cooled to 0-5°. The precipitated dipotassium naphthalate is separated by filtration, washed with 150 ml. of methanol, and dried in a vacuum oven at 150°/150 mm. The dried cream-colorcd salt weighs 130 135 g. (88 92%). 

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