THE USE OF ION-EXCHANGE CHROMATOGRAPHY IN THE ACTIVATION ANALYSIS OF MICROIMPURITIES IN SILICA

Journal Article · Wed Nov 01 04:00:00 EST 1961 · Doklady Akad. Nauk S.S.S.R.

OSTI ID:4821121

Kalinin, A I; Kuznetsov, R A; Moiseev, V V; Murin, A N

The silica sample and several standards of various elements were irradiated simultaneously in a reactor. Various inert carriers (l0 mu g of each element) were added to the silica sample after irradiation. The silica sample was decomposed (n a mixture of HNO/sub 3/ and HF, and evaporated several times almost to dryness with an HF excess. The HF solution containing the induced activities was then rassed through the fluoride form of the strongly-basic anion exchanger AV-l7 (8 to l0% cross-linked with divinylbenzene, grain size 30 to 40 mu , height of column 5 cm, diameter of column 2 mm). The elements Cu(II), Co(II), In(III), Ga(lII), Zn(Il), Cd(Il), and Hg(Il) are not absorbed by the anion exchange in the fluoride form and pass through the column. The mixture of these elements is converted to chlorides, and the elements are separated by eluting with ?rious concentrations of HCl from an anion exchanger in me chloride form according to the scheme proposed by -raus and Nelson. The elements forming negative fluoride omplexes that are absorbed on the AV-l7 anion exchanger in the fluoride form are M(IV), Mo(VI), W(VI), As(V), Ta(V), Sb(V), and Au(IIl). The As, W, Mo, and Sn are eluted together with 17 N HF, and are then separated on a AV-l7 anion exchanger in the chloride form, from which the As is rst eluted with ll.6 N HCl the W with 8 N HCl + l N HF, me Mo with 1 N HCl and the Sn with 2 N HCl +3N HF. Then, the element Ta is eluted from the fluoride anion exhanger with l N HF + 2 N NH/sub 4/NO/sub 3/. Antimony is eluted with 3 N HClO/sub 4/, and finally gold is eluted with l N (NH/sub 2/) /sub 2/ CS (thiourea) which forms a strong complex with gold. Most of the activities are radiochemically pure. The im purities found in a silica sample irradiated for l0 hours at a flux of l0/sup 14/ neutrons/cm/sup 2/-sec vary from 4.1 x l0/sup -8/ wt.% for Au, 4.8 x l0/sup - 8/ wt.% for W and 5.l x l0/sup -8/ wt.% for Hg to 5.9 x l0/sup -5/ wt.% for Sn, 2.8 x l0/sup -5/ wt.% for Sb, and l.8 x l0/sup -6/ wt.% for Mo. The time required for a complete analysis is about 4 hours. (TTT)

• Research Organization: Inst. of the Chemistry of Silicates, Academy of Sciences, USSR; Leningrad State Univ.
• NSA Number: NSA-16-006377
• OSTI ID: 4821121
• Journal Information: Doklady Akad. Nauk S.S.S.R., Journal Name: Doklady Akad. Nauk S.S.S.R. Vol. Vol: 141
• Country of Publication: Country unknown/Code not available
• Language: Russian

Related Subjects

ACIDITY
ACTIVATION ANALYSIS
ADSORPTION
AMMONIUM COMPOUNDS
ANIONS
ANTIMONY
ASTATINE
BENZENE
CADMIUM
CHEMICAL REACTIONS
CHEMISTRY
CHLORIDES
CHROMATOGRAPHY
COBALT
COMPLEXES
COPPER
CROSS- LINKING
DECOMPOSITION
DISTRIBUTION
EVAPORATION
EXTRACTION COLUMNS
FLUORIDES
GALLIUM
GOLD
GRAIN SIZE
HYDROCHLORIC ACID
HYDROFLUORIC ACID
IMPURITIES
INDIUM
INDUCTION
ION EXCHANGE
ION EXCHANGE MATERIALS
IRRADIATION
MERCURY
MIXING
MOLECULES
MOLYBDENUM
NEUTRONS
NITRATES
NITRIC ACID
ORGANIC SULFUR COMPOUNDS
PERCHLORIC ACID
POLYMERIZATION
QUANTITY RATIO
REACTORS
SAMPLING
SEPARATION PROCESSES
SILICON OXIDES
SOLUTIONS
STANDARDS
TANT