Chromium gravimetric analysis

Cadmium and inorganic compounds of cadmium in air (X-ray fluorescence spectroscopy) Chromium and inorganic compounds of chromium in air (atomic absorption spectrometry) Chromium and inorganic compounds of chromium in air (X-ray fluorescence spectroscopy) General methods for samphng and gravimetric analysis of respirable and inhalable dust Carbon disulphide in air... 

Methods. Polyamic acid in NMP was spin-coated onto a Si or Quartz wafer (diameter = 2.25 inches) coated with Cr, and then cured to polyimide at 400 °C. The purpose of the 500-750-A-thick layer of chromium is to enhance wettability and to give good reflectance to the Quartz wafer. Kapton H (PMDA-ODA) and Upilex S (BPDA-PDA) films were employed for gravimetric analysis. Around 5-um thick layers were used to measure the thickness change. The 100-1000-A-thick layers were employed to obtain XPS and ER IR spectra. The samples for contact angle measurement, XPS and ER IR were dried under vacuum at ambient temperature for 12-24 h and the samples for gravimetric analysis were dried at 85 °C for 12 h. The samples for film thickness measurement were fully re-cured to polyimide. 

In gravimetric analysis, the solution-preparation step has its own special significance. The analyte must be separated from interfering species, or the interferents must be masked. For example, if iron(III) is to be estimated as its hydrated oxide in the presence of chromium(III), then the mixture is initially treated with perchloric acid so as to oxidize chromium(III) to chromate (chromium(VI), Cr04 ), followed by addition of ammonia to precipitate the hydrated iron oxide. Sometimes it is necessary to remove interferents, for example, when calcium is to be estimated as calcium sulfate in the presence of barium. The barium is removed as its chromate and the calcium is precipitated quantitatively as its sulfate. 

Estimation of Chromium.—In the analysis of chromites or of other substances containing chromium, such as leather ashes, pigments, etc., it is first necessary to obtain a solution. This is done by finely powdering the substance and heating it with a suitable flux in a crucible, preferably of nickel. Many fluxes have been employed, usually caustic alkali or alkali carbonates, but the one in most common use at present is sodium peroxide, whereby the chromium compound is rapidly converted to a chromate. - Excess of alkali is removed by boiling with ammonium carbonate, which also precipitates any iron present. The filtrate is then acidified with dilute sulphuric acid and the chromium estimated either by gravimetric or volumetric methods. 

---