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An Alkaline Solution of Potassium Chromate As a Transmittancy Standard in the Ultraviolet G Eraldine W

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An Alkaline Solution of Potassium Chromate As a Transmittancy Standard in the Ultraviolet G Eraldine W Journal of Resea rch of the National Bureau of Sta ndards Vol. 48, No. 12, June 1952 Research Paper 2331 An Alkaline Solution of Potassium Chromate as a Transmittancy Standard in the Ultraviolet G eraldine W. Haupt The need for a means of testing t.he reliability of t he photometric scale of spectro­ photometers in the ultraviolet region (where glasses are unsuitable) h as led to t. he study of an aqueous solution of potassium chromate havin g t he composit ion 0.0400 g/li ter of K2Cr04 in 0.05 N KOH. Based on extensive measurements, llsing photogra phic, photo­ electric, a nd visual spectrophotometry , standard values of spectral t ra nsmittancy have been determined for 1.000 and 2.000 cm of solution at 25° C from 220 to 500 mIL . These values have been tabulated alo ng wit h derived values of absor bancy, molar a bso rbancy indcx a M, a nd 10glOaM. The latter values have been compared graphicall y wit h those of ot her observers . Changes in spectr al transmittancy with changes in temperature have been determined. The work has also included a study of the e ffects due to t he contain er bottle and to age of solut ions over periods up to 8 years, and a co mparison of results ob­ tained with t he solution prepa red either from K 2Cr04 or from l(2C r20 7 as one of t he reagents. 1. Introduction To make the solution most useful as fl calibration standard of spectral transmittancy in the ul traviolet, A means of testing the r eliability of the photo­ information should be availahle r egarding its per­ metric scale of spectrophotometers in the ultraviolet manence, or stability. under specified conditions region has been in demand fo r a number of years. (including the effects of the container bot tles on the With the introduction of commercial photoelectric spectral transmittancy) and regarding any change in spectrophotometers for the ul traviolet in 1940, the its spectral transmittancy with tempera ture over the demand increased considerably. range of room temperatures to be expec ted . Such Although glass fil ter standards of spectral trans­ data have accordingly been obtained . mittance [1, 2] I have proved to be a very sa tisfac­ This investigation was star ted in 1940 and discon­ tory and valuable means of testing the reliabIlity of tinued in 1943 because of the war . I t was resumed the photometric scale of spec trophotometers in the in 1948, and preliminary data have been published visible region, they are in general unsatisfactory in [8, 9. 10]. The presen t paper describes the work the ultraviolet. Not only do all but a few special leading up to the determination of these preliminary glasses absorb completely below 290 m/-L , but, in values, based solely on the measuremen ts made in addition, the ultraviolet spec tral transmittances of 1940- 43, and describes the recen t work on new solu­ many glasses change on exposure to strong ultra­ tions with a new instrumen t, on the basis of which violet radiant flu x [2, 3, 4] . In these respects solu­ the final values were derivecl as herein published . tions in cells with quartz end plates are found to be superior to glasses for use in the ultraviolet. In 2. Preparation of Solutions addition, solutions are reproducible and can be pre­ pared in the laboratory from specifications with All the potassium clu'omate solutions studied were relatively small time and cost. Various solutions prepared in the Bureau's Chemistry D ivision by have been studied or recommended 23 for this pur­ W. Stanley Clabaugh . The solutions are of two pose. Preeminen t among these is an aqueous solu­ general types (A) those prepared bv dissolving the tion of potassium chTomate, K 2Cr04 (0.04 g/liter) in salt in dilute solution of KOH, and (B ) those prepared 0.05 N KOH. This has alternate regions of high by dissolving the sal t in distill ed water. transmission and absorption in the ultraviolet, and The type (A), or alkaline, solutions were prepared this one solution in 1- and 2-cm thicknesses covers as follows: the transmittancy scale from abou t 0.90 to about (AI): A solution of K2Cr0 4 stock material, rea­ 0.01 (0.046 to 2. 0 in absorbancy). Several investi­ gent, grade, 0.0400 g/liter, in 0.05 N KOH (solution gators have previously worked with this solution, of potassium hydroxide prepared by dissolving 3.3 g and from the information available in 1940 this ap­ of potassium hydroxide sticks (Sfi% KOH) of reagent peared to be one of the best fo r the purpose. It was These solu tions havc their limitations fo r use as calibration standards both in accordingly selected for calibration .4 the shortwave end. of the visi ble region and in the ultraviolet region. In the visible, neither of them has sufflcient absorption in the violet to be of much value 1 Figures in brackets indicate the literature refe rences at the end of this pa pcr. for the purpose. I u the ultraviolet, the copper sulfate solu tion varies rather 2 For example, Brode 15, p. 2001 lists potassiu m chromate, azo benzene, and ra pidly from high transparency at wavelen gths above 330 m" to high absorption potassium n itrate as solutions that can be accurately prepared as standards for at wavelengths below 270 m}.L and thus has no general utility over the whole the calibration of spectrophotometers. region . rrhc co balt ammonium sulfate solution used in the D avis-Gibson filters 3 P hotoelectric Spectrophotometry Group of England has recently conducted [7] has too hi gh transparency between 230 and 400 m" to be of much value as a a collaborative test on the use of 1(,C1"2 0 , [61. gpectrophotometric stalld~rd . Solntiolls prepared at 10 times this co ncentration 4 Solution s can, of co urse, also be used in the visible region. In fact, the aq ueous werc fo und (un published d~ta) to be unstable with time throughout the ultra· solutions of copper sulfate and cobalt ammonium sulfate used in the Davis·Gibson violet and were thus considered undesirable for usc as spectrophotometric filters [7, 8, 9, 101 have been recommcnded for that purpose. ca li bration stand3.rds. 414 quality in sufficient distilled wat!'!' to make 1 liter). 3.1. Photographic Method (A2 ): A solution of K 2CrO'1 of the same concen­ tration and alkalinity as (AI) but prepared from TIIC photographic data were obtained by means of 0.0303 g of K 2CrZ07 5• which, when converted gave til e Hilger sector photometer with th e Fues quartz 0.0400 g of K zCr04/liter. This follows from the spectrograph [11 , 12, 13]. reaction K2Cr207 + 2KOH= 2KzCr04+ H zO. The equivalent slit widths for an 0.2-mm sli t, The purpose of clissolving the potassium chromate \Vh ich was used throughou t all th e exposures, arc in dilute solutions of KOH was to prevent any di­ chromate from forming. In A2 a potassium chro­ mate solu tion was prepared by means of a different \\Ta velength I Slit widths material, potassium dicID'omate. Tills solution was preparod to determine whether the spectrophoto­ 'lnj1. IIWI /11,!" metric data from Al and A2 would be identical. 400 O. 2 O. 6 Since they were found to be identical, there is a 310 . 2 . 25 260 .2 . 13 distinct advantage in using potassium dichromate as 220 . 2 . 08 one of the reagents rather than potassium chrol11 ute, because in stock material potassium dichromate exists in a purer state. A special sample of potassium On each plate exposures were made of at lea t two chromate that had been r ecrystallized four times was aluminum spark spectra for wavelength calibration used in the preparation of one of the B, or neutral, purposes. A calibration curve was used to translate solutions with the view to studying the effect of the scalar valu es, which were read at th e density mateh­ puri ty of the potassium chromate. poin ts, into wavelengths. Both 1.000- and 4.000-cm The solutions prepared in 1940, 1942, and again in cells were used wi th th e H il ger instrument. 1949 were stored in liter bottles of the ordinarv storeroom glass type with glass stoppers. For fm:­ 3.2. Visual Method ther study of the effect of storage, half of the 1940 alkaline solu tion prepared from K2Cr04 and half of The Konig- Martens spectrophotometer [13 , 14] is the 1940 neutral solu tions were stored in similar a visual instrument. The slit wid ths lI sed on this bottles lined with ceresin. The tips of the l"ll bber instrument are varied, depending upon th e wave­ stoppers used were also covered with ceresin. Also length and th e spectral ch aracteristics of th e sample half of the alkaline solutions prepared by methods At being measured. With an incande cent so urce th e and A2 in 1949 were stored in alkali-resistant g l as~ equivalent slit widths in millimicrons used for two (Corning glass 728) . wavelengths and for two settings of the sli ts ar c N one of the solu tions was exposed to light excep t given below: when actually in use to fill the cells for their measure­ I ment. No solution was ever poured out of its bottle. Wavelength Slit widths In filling th e cell s a pipette was used to draw off the solution.
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