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1.
Conditions were found under which manganese(III) acetate can be electrochemically generated at a platinum anode with 100% current efficiency. It was found that even traces of
Time (min) | 0 | 5 | 10 | 30 | 60 | |||
Consumption of Mn(III) (mol/mol) | 2.00 | 1.99 | 2.00 | 2.01 | 2.00 |
SO2 (ppm) | ?HgCl2a | ?HgBr2 | ?Hg(Ac)2b | ?Hg(SCN)2 |
2.0 | 12,500 | 10,000 | 10,000 | 9,200 |
4.0 | 12,500 | 11,500 | 10,000 | 9,000 |
6.0 | 12,500 | 11,500 | 10,000 | 9,200 |
8.0 | 12,000 | 11,000 | 10,500 | 9,800 |
- a
- Molar absorptivity based on sulfite ion at 230 nm. Solution was 6.86 buffer.
- b
- Mercuric acetate solutions seemed to be somewhat unstable. absorptivity of about 25,000. The absorbance is linear over a range of approximately 0.5–5.0 ppm as SO2. Covalent mercury(II) compounds form a complex with sulfite, Hg(SO3)22?, which absorbs at 230 nm and shows a linear response over a range of 1–8 ppm as SO2.
3.
A sensitive spectrofluorimetric procedure with rhodamine B in the presence of aluminum chloride is given for determining submicrogram and microgram quantities of thallium in silicate rocks. Samples are decomposed with a mixture of hydrofluoric and nitric acids and then treated with hydrochloric acid. Thallium is extracted as its dithizonate with chloroform from an alkaline medium containing ascorbate, citrate, and cyanide and then back-extracted with dilute nitric acid. After destruction of the organic matter and treatment with bromine, hydrochloric acid, aluminum chloride, and rhodamine B, the
相似文献
Thallium (p.p.m.) | Method | Ref. | |
G-1 | W-1 | ||
1.06 | 0.102 | Neutron activation analysis | 1 |
1.08 | 0.121, 0.116 | Neutron activation analysis | 2 |
1.3 | 0.17 | Neutron activation analysis | 3 |
1.3 | 0.11 | Spectrographic | 4 |
0.105–0.110 | Flameless atomic absorption spectroscopy | 5 | |
1.3a | 0.13a | 19 | |
1.24b | 0.110b | 20 | |
1.09 ± 0.01 | 0.110 ± 0.005 | Spectrofluorimetric | Present method |
- a
- Values given by Fleischer.
- b
- Average value given by Flanagan. fluorescence intensity of the benzene-extracted rhodamine B chlorothallate is measured. The limit of determination is approximately 0.01 p.p.m. for a 1.0-g sample. The thallium contents of U.S. Geological Survey standard rocks G-1 and W-1 were found to be 1.09 ± 0.01 and 0.110 ± 0.005 p.p.m., respectively.
4.
A simple, rapid, and accurate method for determination of total sulfur and inorganic sulfate in biological materials by barium chloranilate colorimetry is presented. Criteria required
Sample | Determinations | Mean (μg) | SD (μg) | |||||
Whole blood | 10 | 1004 | 21 | |||||
Blood plasma | 10 | 543 | 4 | |||||
TCA extracts | 10 | 24 | 2 | |||||
Urine (totals) | 10 | 598 | 31 | |||||
Urine (inorganic S) | 10 | 374.4 | 19 |
Transition metal | Concentration (M) | Percentage inhibition | Mg(II) found (×l05M) |
Fe(II) | 3.6.10?5 | 54.1 | 4.62 |
Fe(III) | 3.6.10?5 | 47.8 | 4.48 |
Co(II) | 3.4.10?5 | 50.0 | 4.53 |
Ni(II) | 3.4.10?5 | 50.0 | 4.53 |
Cu(II) | 3.1.10?5 | 52.0 | 4.56 |
Zn(II) | 3.0.10?5 | 54.1 | 4.62 |
Cd(II) | 1.7.10?5 | 52.0 | 4.56 |
Hg(II) | 9.9.10?6 | 45.8 | 4.44 |
Sn(II) | 2.1.10?6 | 50.0 | 4.52 |
Pb(II) | 1.2.10?6 | 54.1 | 4.62 |
- a
- Conditions: 4.53.10?5M Mg(II), 35 ng Mn ml?1, 0.429 M ammonia, 1.6.10?4M OH-PDT.
Mg(II) found (M)b | |||
Natural water | Ca(II) presenta | Atomic absorption | |
sample | M | Kinetic absorption | method |
Commercial | 3.45 · 10?4 | 1.65 · 10?3 | 1.74 · 10?3 |
Commercial | 5.46 · 10?4 | 1.57 · 10?4 | 1.81 · 10?4 |
Untreated | 6.13 · 10?4 | 2.16 · 10?4 | 2.40 · 10?4 |
Treated | 4.95 · 10?4 | 1.93 · 10?4 | 2.17 · 10?4 |
- a
- EDTA titration less the magnesium.
- b
- Average of three separate determinations. traces of magnesium(II). The reaction is followed spectrophotometrically by measuring the rate of change in absorbance at 594 nm. The calibration graph (percentage inhibition vs magnesium concentration) is linear in the range 329–535 · 10?5M with an accuracy and precision of 1.2%. The method has been applied to the determination of magnesium in natural waters at low concentrations.
6.
Cadmium ions react with the collector, ethylhexadecyldimethylammonium bromide (EHDABr), to form a surface-active sublate which can be removed from aqueous bromide
相似文献
Foreign ion | Foreign ion concentration (M) (×10?5) | Foreign ion removed (%) | Cadmium removed (%) |
None | 99.21 | ||
Zn2+ | 6.11 | 0.06 | 98.41 |
Cu2+ | 6.29 | 3.64 | 97.80 |
Pb2+ | 3.86 | 4.80 | 91.78 |
Cr6+ | 7.69 | 30.75 | 99.07 solutions by ion flotation. A typical ion flotation procedure involves passing air through a 250-ml solution containing 5 ppm Cd2+, 0.05 M Br?1, and 1.7 × l0?3M EHDABr at a flow rate of 40 ml/min for 1 hr. The procedure was simple and efficient. Chromium, copper, and zinc ions do not interfere under the experimental conditions. |
- a
- Cd2+, 4.46 × 10?5M; EHDABr, 4.25 × 10?4; Br?, 5 × 10?2M; flow rate, 40 ml/min; time, 60 min.
7.
Spectrophotometric investigation of the deep blue colored, water-soluble complex of
Method | ΔF (Kcal/mole) | |||||||
Mukherji and Dey (4) | 4.11 | ?5.70 | ||||||
Subhrana and Raghavrao (6) | 4.80 | ?6.66 |
Perchlorate | Nitrate | |||||||
Taken (μg) | Found (μg) | Error (%) | Taken (μg) | Found (μg) | Error (%) | |||
400 | 404 | + 1.00 | 248 | 250 | +0.81 | |||
400 | 400 | 0.00 | 496 | 492 | ?0.81 | |||
400 | 400 | 0.00 | 992 | 992 | 0.00 | |||
800 | 796 | ?0.50 | 248 | 248 | 0.00 | |||
600 | 602 | +0.33 | 248 | 245 | ?1.21 | |||
800 | 792 | ?1.25 | 496 | 498 | +0.40 |
Hydrochloric acid | 4 — 8M | |||||||
Lead | 0 — 0.03M | |||||||
Antimony | 0 — 0.002M |
Cell type | Applications | |||||||
Human polymorphonuclear leukocytes | (1) Detection of bactericidal defects, particularly chronic granulomatous disease | |||||||
(2) Detection of host opsonic defects (both immunoglobulin and complement ?C3b opsonic defects). | ||||||||
(3) Analysis of drug effects on host cellular and opsonic defenses (9,11). | ||||||||
(4) Characterization of bacteria or other particulate matter in terms of ability to generate opsonic activity and/or be ingested by phagocytic cells (3,7). | ||||||||
Alveolar macrophages | (1) Detection of environmental pollutant effects on respiratory defense mechanisms (against both particulate and soluble matter). | |||||||
(2) Analysis of drug effects on respiratory defense mechanisms, particularly drugs administered in the treatment of respiratory diseases. |
pK1 | pK2 | |||||||
2,3-butanedionedioxime | 10.6 ± 0.1 | 11.9 ± 0.3 | ||||||
1,2-cyclohexanedionedioxime | 10.6 ± 0.2 | 12.4 ± 0.5 | ||||||
1,2-cycloheptanedionedioxime | 10.7 ± 0.2 | 12.3 ± 0.5 |
Constituents | Thorn Smith # 30 | Thorn Smith # 54 | NBS # 37E | NBS # 63C | ||||
Cu present | 59.30 | 84.04 | 69.61 | 80.48 | ||||
Zn | 37.81 | 1.452 | 27.85 | 0.093 | ||||
Pb | 0.1 | 8.590 | 1.00 | 9.35 | ||||
Sn | Trace | 5.737 | 1.00 | 9.03 | ||||
Sb | 0.52 | |||||||
Ni | Trace | 0.53 | 0.32 | |||||
P | 0.145 | |||||||
S | 0.060 | |||||||
As | 0.023 | |||||||
Fe | 1.22 | 0.004 | 0.0013 | |||||
Al | 1.15 | |||||||
Mn | 0.35 | |||||||
Cu found | 59.09 | 83.64 | 69.68a | 80.54a | aAverage of 3 determinations. |
isotope | -B0 (MHz) | DJ (kHz) | xN1 (MHz) | xN2 (MHz) | ||||
HC14N-HC14N | 1745.80973(50) | 2.133(30) | ?4.0973(200) | ?4.4400(190) | ||||
HC14N-HC15N | 1700.30190(30) | 1.939(40) | ?4.1059(10) | - | ||||
HC15N-HC14N | 1729.92082(20) | 2.023(30) | - | ?4.4339(6) | ||||
HC15N-HC15N | 1684.28825(25) | 1.900(30) | - | - |
Thiosemicarbazone | Log | |||||||
-Benzaldehyde | 15.5 ± 0.1 | |||||||
-Picolinaldehyde | 14.0 ± 0. | |||||||
-6-Methylpicolinaldehyde | 14.5 ± 0. | |||||||
-Salicylaldehyde | 15.7 ± 0.1 | |||||||
-p-Hydroxybenzaldehyde | 15.6 ± 0. | |||||||
-p-Dimethylaminebenzaldehyde | 17.2 ± 0.1 |
Hydroxide by ammonium hydroxide | 408° | |||||||
Hydroxide by ammonia | 400° | |||||||
Hydroxide by urea | 475° | |||||||
Hydroxide by aniline | 546° | |||||||
Hydroxide by sulpliitc | 813° | |||||||
Hydroxide by tannin | 520° | |||||||
Cupfcrron | 745° | |||||||
Camphoratc | 478° | |||||||
Dibromo-oxinate | 817° |
Strippant | Cobalt stripped (%) | |||||||
Na2S (M) 1.0 | 18.3 | |||||||
2.0 | 10.7 | |||||||
Na2SO3 (M) 0.1 | 10.7 | |||||||
0.5 | 49.6 | |||||||
1.0 | 52.9 | |||||||
EDA (%) 2.5 | 76.6 | |||||||
NaOH (M) 0.1 | 4.1 | |||||||
0.5 | 74.1 | |||||||
1.0 | 90.8 | |||||||
2.0 | 76.8 | |||||||
NH4OH (M) 0.1 | 24.1 | |||||||
0.5 | 91.8 | |||||||
1.0 | 97.5 | |||||||
2.0 | 99.9 | |||||||
EDTA (M) 0.02 | >99.9 | |||||||
0.05 | >99.9 | |||||||
0.1 | >99.9 | |||||||
EDTA (%) 0.1 | >99.9 | |||||||
0.5 | >99.9 | |||||||
1.0 | >99.9 |
A | B | C | ΔJ | ΔJK | ||||
(CH2)O3?HF | 9217 | 2575.1 | 2350.6 | 11.3 | ?57.0 | |||
(CH2)3O?DF | 9157(ass) | 2544.7 | 2329.3 | 9.9 | ?56 |
Hydroxide by ammonia | 345° | |||||||
Hydroxide by hexamethylene tetramine | 546° | |||||||
Hydroxide by cyanate | 475° | |||||||
Sulphide | 94–221°, 320–544°, 690° | |||||||
Phosphate | 477° | |||||||
Luteocobaltic indichloride | 100–105° | |||||||
Oxinate | 100–285° | |||||||
Diethyldithiocarbamate | 100–210° |
CaCO3 (mg) | C (mg) | Flow rate (cm3/min) | C found (mg) | C (%) | ||||
27.989 | 3.359 | 100 | 3.3669 | 12.03 | ||||
28.604 | 3.432 | 200 | 3.4343 | 12.00 | ||||
29.259 | 3.511 | 300 | 3.5149 | 12.01 | ||||
33.808 | 4.057 | 400 | 4.0381 | 11.94 | ||||
5.629 | 0.675 | 500 | 0.6760 | 12.01 | ||||
10.311 | 1.237 | 500 | 1.2337 | 11.96 | ||||
15.647 | 1.878 | 500 | 1.8706 | 11.95 | ||||
35.214 | 4.226 | 500 | 4.1982 | 11.92 | ||||
40.733 | 4.888 | 500 | 4.8212 | 11.84 | ||||
59.678 | 7.161 | 500 | 7.0263 | 11.77 | ||||
30.386 | 3.646 | 780 | 3.5941 | 11.83 | ||||
29.781 | 3.574 | 780 | 3.5361 | 11.87 | ||||
28.113 | 3.374 | 1150 | 3.2534 | 11.57 |
Element | Increment no.20 (1832–1838) | Increment no.8 (1932–1838) | Increment no.3 (1858–1863) | Increment no.1 (1868–1872) | ||||
Core Number | Core Number | Core Number | Core Number | |||||
1 | 3 | 1 | 3 | 1 | 3 | 1 | 3 | |
Na | 12.9(1.1) | 2.67(3.3) | 33.8(1.0) | 11.2(1.6) | 15.6(1.5) | 31.4(1.2) | 22.4(0.93) | 9.9(1.8) |
Mg | c | c | 160(12)b | 80(27)b | 100(21)b | 100(30)b | c | c |
Al | 15.2(5.4) | 5.6(6.1) | 12.5(3.8) | 11.0(4.4) | 7.8(6.6) | 8.4(7.4) | 6.5(14) | 6.6(6.2) |
Cl | 15.4(9.1) | ND | 66(5.4) | ND | ND | 55(6.1) | 26(5.5) | 22(5.1) |
K | 205(2.6) | 223(3.3) | 493(1.8)b | 457(1.9)b | 478(1.9)b | 439(2.1)b | 449(1.8) | 570(1.7) |
Ca | 1600(11) | ND | ND | ND | ND | ND | ND | ND |
Cr | ND | ND | NDb | NDb | 0.3(>30)b | 0.6(>30)b | 0.6(>30)b | ND |
Mn | 109(0.30) | 107(0.23) | 64.1(042) | 108(0.32) | 46.7(051) | 66.8(0.44) | 38.9(0.39) | 45.0(0.34) |
Fe | ND | ND | ND | ND | ND | 19(19) | 25(18) | ND |
Co | ND | 0.02(>30) | ND | ND | ND | ND | 0.30(>30) | ND |
Zn | 7.2(7) | 7.4(4.2) | 13.0(2.4) | 9.2(3.3) | 5.6(4.0) | 4.5(4.7) | ND | 2.4(8.8) |
Br | 0.10(20) | ND | 0.07(12) | ND | 0.024(13) | ND | 0.04(>30) | ND |
Rb | ND | ND | 0.9(13) | 0.8(18) | 0.8(15) | 0.7(17) | ND | 1.1(18) |
Ag | ND | ND | 1.06(3.0) | 15.3(0.71) | 0.15(15) | 0.69(4.8) | 0.11(28) | ND |
Ba | 11(7.3) | 10(13) | 3.2(16) | ND | 3.0(15) | 2.9(18) | ND | 3(32) |
W | ND | ND | ND | ND | ND | ND | 0.06(29) | ND |
- a
- Results in p.p.m followed by (per cent counting statistical error).
- b
- Computer forced result.Also V,Se,Sr,Sb,Cs and au (forced) were not detected.
- c
- Element possibly present but missed by peak-finding routine.7 35–45, was used in developing an instrumental absolute multielement method. The detector was calibrated for absolute counting with two independent sets of radioactivity standards for four detector- -source distances; the absolute activities of the standards were reproducible within accuracies of 9%. Five sources of systematic error were investigated: (a) correction for counting of cylindrical sources for 26 γ-ray energies reached 14–17% for photon energies below 500 keV; (b) flux variation during bombardment and within the irradiation capsule volume was not significant; (c) samples were sufficiently stable during high-flux bombardment; (d) multi-element impurities in accessory materials (polyethylene and “Nucleopore” filters) were not significant; (e) correction for sample activation during rabbit transfer was necessary for short bombardments, e.g., 8.6 % for 6 s and 19.6 % for 4 s. This methodology resulted in accuracies of 10–15 % for most elements, as determined by analysis of N.B.S. orchard leaves and coal and of Bowen's kale standards. The method was applied to a preliminary chronological study of environmental baselines and contamination levels, based on tree ring samples, covering a period of 100 years.
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