1367.1 GOST-83
STATE STANDARD OF THE USSR
ANTIMONY
SPECTRAL METHOD OF DETERMINATION OF IMPURITIES
WITHOUT PRIOR ENRICHMENT
Antimony. Spectral method for the determination of
impurities without preliminary concentration
1367.1 GOST-83
Group B59
AXTU 1709
Replace GOST 1367.1−76
The validity of
from January 1, 1985
before January 1, 1990
This standard specifies the emission spectral method for the determination of lead, arsenic, iron, tin, silicon, zinc, bismuth, gold, Nickel, copper, cadmium, magnesium, manganese and silver without prior enrichment in antimony.
The method is based on the intensity of spectral lines of lead, arsenic, iron, tin, silicon, zinc, bismuth, gold, Nickel, copper, cadmium, magnesium, manganese and silver content of these elements in the antimony in the excitation of these elements in the arc either AC or DC.
The emission spectral method without pre-enrichment allows to determine the mass fraction of impurities in the antimony, %:
lead from
arsenic from
iron from
tin from
silicon from
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
of zinc from
of bismuth from
gold from
Nickel from
copper from
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
of cadmium from
of magnesium from
manganese from
silver from
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis and security requirements — according to GOST 1367.0−83.
2. APPARATUS, MATERIALS AND REAGENTS
The diffraction type spectrograph DFS-8 with grille 600 strokes at 1 mm or another similar device.
The quartz spectrograph medium dispersion type of ISP-30 or other similar device.
Microphotometer geregistreerde type MF-2 or another similar device.
A constant current source providing a voltage of at least 200 In and designed for a current of 20 A.
Generator activated arc type DG-2, DG-1, PS-39 for ionization of the interelectrode gap at the time of switching arc DC or AC, calculated in the latter case, current up to 20 A.
The infrared lamp of SCP-500 on the other 16−87 IFMR.675000.006 the voltage regulator RNO-250−0,5 or controller of the same type.
(paragraph added by the Change in N 1, approved. By the decree of Gosstandart of the USSR from
Grinding machine graphite electrodes with a speed of up to 1420 rpm.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
The graphite electrodes of 6 mm in diameter marks-2 or high purity-7−4 a simple form with a crater diameter of 4 mm and a depth of 8 mm and with a crater diameter of 4 mm and a depth of 4 mm.
Electrodes in the form of «glasses» made of graphite marks-2 or high purity-7−4 (Fig. 1).
Damn. 1
Contradictory of graphite rods stamps-2 or high purity-7−4 with a diameter of 6 mm, length 30 — 50 mm, one end of which is confined to the hemisphere.
The graphite powder of high purity according to GOST 23463−79 or obtained from graphite electrodes high purity-7−4.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
Photographic plates of the spectral type of ES sensitivity of at least 10 units according to GOST 10691.6−88 or type II sensitivity not less than 15 conditional units according to GOST 10691.6−88, or photographic plates of the same type, providing a normal blackening of analytical lines and the background in the spectrum.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
Photographic plates of the spectral type ø sensitivity not less than 8 units according to GOST 10691.6−88 or photographic plates of the same type, providing a normal blackening of analytical lines and the background in the spectrum.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
The developer according to GOST 10691.1−84.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
Fixer: 300 g chernovetskogo sodium (GOST 27068−86) and 20 g of ammonium chloride (GOST 3773−72) was dissolved in 700 and 200 cm3 of water respectively, the resulting solutions merge together and adjusted with water to 1 dm3.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
Weighing accuracy of 0.1 g. photoreactive
Analytical scale.
Buxy of organic glass.
Mortar, agate, Jasper organic glass pestle of the same material.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
Spatulas made of organic glass.
Organic glass funnel for loading samples into the crater of the electrode (Fig. 2).
Damn. 2
Trays-plastic or plastic with lids with capacity of 50 — 100 cm3 sample storage comparison.
Lead oxide on the other 6−09−5382−88.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
Arsenic anhydride according to GOST 1973−77.
Iron oxide on the other 6−09−5346−87.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
Tin dioxide according to GOST 22516−77.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
Silicon dioxide according to GOST 9428−73.
Zinc oxide according to GOST 10262−73.
Bismuth oxide according to GOST 10216−75.
Gold metal according to GOST 6835−80.
Nickel oxide according to GOST 4331−78.
Copper oxide under GOST 16539−79.
Cadmium oxide according to GOST 11120−75.
Magnesium oxide according to GOST 4526−75.
Manganese (IV) oxide according to GOST 4470−79.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
Silver nitrate according to GOST 1277−75.
Ethyl alcohol GOST 18300−87.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
A sample comparison: antimony grades Su00000 or Su0000p, checked in their spectra the lines of the determined elements: arsenic, tin, silicon, and gold — according to GOST 1367.1−83, lead, iron, zinc, bismuth, Nickel, copper, cadmium, magnesium, manganese and silver — GOST 1367.2−83.
Standard solution gold: 200 mg of metallic gold dissolved in 30 cm3 of Aqua Regia (1 part nitric acid and 3 parts hydrochloric acid) under moderate heating to complete dissolution of gold.
The solution was transferred to volumetric flask with a capacity of 100 cm3 and adjusted to the mark with distilled water, mix thoroughly.
1 cm3 of solution contains 2 mg of gold.
3. PREPARATION FOR ASSAY
3.1. Sample preparation comparison
The main reference sample (OOS) is prepared by introduction of antimony brand Su00000 or Su0000p selected according to sec. 2, the analyzed impurities in the form of oxides or salts.
Prepare the main reference sample (OOS) containing 1% mass fraction of lead, arsenic, iron, tin, silicon, zinc, bismuth, gold, Nickel, copper, cadmium, magnesium, manganese and silver: in an agate or a Jasper mortar placed 807,9 mg of antimony brand Su00000 or Su0000p in the form of powder with particle size less than 0,074 mm and the first drops add 5 cm3 of a standard solution of gold (10 mg) at a constant drying under an infrared lamp. Then to the mixture was added 10.8 mg of lead oxide, 13,2 mg of arsenious anhydride and 14.3 mg of iron oxide, of 12.7 mg of tin dioxide, 21,4 mg of silicon dioxide, 12.5 mg of zinc oxide, 11.1 mg of bismuth oxide, 14,1 mg of Nickel oxide, 12.5 mg of copper oxide, 11.4 mg of cadmium oxide, 16,6 mg of magnesium oxide, 15.8 mg of peroxide of manganese, and 15.7 mg of silver nitrate and triturated with ethylalcohol to obtain a homogeneous mixture.
References OS1 and ОС13 prepare a serial dilution of wasps, and each subsequent sample SB brands Su00000 or Su0000p selected according to sec. 2.
The mass fraction of each of the designated impurities in samples OS1 — ОС13 and added to the mixture of the antimony sample and diluted sample, mixing to obtain the subsequent sample, are given in table. 1.
Table 1
────────────┬────────────────┬────────────────────────────────────
Designation │ Mass fraction │ Mass of test portions, g
sample │ defined├─────────────┬──────────────────────
│ impurities, % │Antimony grades │Dilute sample
│ │ Su00000 or │(in brackets it
│ │ Su0000p │ designation)
────────────┼────────────────┼─────────────┼──────────────────────
│ -1 │ │
OS1 │3 x 10 │1,400 │0,600 (EP)
│ -1 │ │
OS2 │1 x 10 │2,000 │1,000 (OC1)
│ -2 │ │
ОС3 │3 x 10 │2,800 │1,200 (OS2)
│ -2 │ │
OS4 │1 x 10 │2,400 │1,200 (ОС3)
│ -3 │ │
ОС5 │3 x 10 │2,800 │1,200 (OS4)
│ -3 │ │
OS6 │1 x 10 │2,400 │1,200 (ОС5)
│ -4 │ │
OS7 │3 x 10 │2,800 │1,200 (ОС6)
│ -4 │ │
ОС8 │1 x 10 │2,400 │1,200 (OS7)
│ -5 │ │
OS9 │3 x 10 │2,800 │1,200 (ОС8)
│ -5 │ │
ОС10 │1 x 10 │2,400 │1,200 (OS9)
│ -6 │ │
ОС11 │3 x 10 │2,800 │1,200 (ОС10)
│ -6 │ │
ОС12 │1 x 10 │2,400 │1,200 (ОС11)
│ -7 │ │
ОС13 │3 x 10 │2,800 │1,200 (ОС12)
Listed in the table. 1 sample of antimony and diluted sample was placed in an agate or a Jasper mortar, ground thoroughly with ethyl alcohol (ОС8 — ОС13 with ethanol, double-distilled in quartz apparatus) for 20 min and dried under an infrared lamp. Grinding in a mortar, and drying under a heat lamp are in buxa of organic glass.
The samples of the comparison is stored in tightly closed cans of organic glass.
3.2. Sample preparation samples and comparison to analysis
The analyzed samples (two sample from each sample of antimony Su00000 brands, Su0000p, Su0000) and comparison samples before analysis mixed in a mortar made of organic glass with graphite powder in the analysis of antimony Su00000 brands, Su0000p and Su0000 ratio of 10:1 by weight (2,000 mg of the sample and 200 mg of graphite powder); in all other cases, in the ratio 4:1 by weight (2,000 mg sample and 500 mg of graphite powder) and poured through a funnel made of organic glass in the craters of the electrodes, prebaked graphite with contractrate in the arc of an alternating current power 15 And for 15 S.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
The coating is compacted by tapping the non-working end of the electrode on the bottom of the box and fill up the analyzed sample to completely fill the crater.
For the analysis of antimony Su00000 brands, Su0000p and Su0000 apply six electrodes in the form of glasses. For the analysis of antimony brands Su000, Su00, su0, SS1 and SS2 apply six electrodes of a simple shape with a crater diameter of 4 mm and a depth of 4 mm.
To determine the mass fraction of zinc, arsenic and cadmium in all brands of antimony used six electrodes of a simple shape with a crater diameter of 4 mm and a depth of 8 mm.
In the analysis of antimony brands Su00, su0, SS1 and SS2 powdered sample of antimony is mixed with antimony brand Su00000 in the required ratio.
The degree of dilution (i.e. the dilution factor equal to the ratio of the mass of the diluted and undiluted analytical samples) are chosen so that the logarithm of the contents defined contaminants (lgC) in dilute a sample of antimony was in the straight portion of the calibration graph built on samples of comparison for this impurity (see section 5.1).
4. ANALYSIS
4.1. Photographing spectra
4.1.1. To determine the mass fraction of lead, iron, tin, silicon, bismuth, gold, Nickel, copper, manganese, magnesium, and silver spectra comparison of samples and analyzing the samples photographed on a spectrograph DFS-8 to the disc type ES or type II using a three-step attenuator and a width of slit of the spectrograph 0,025 mm.
The slit of the spectrograph light being a condenser, the notch height of the intermediate diaphragm, the image of which is recorded in the process of arc burning in the interelectrode gap, 5 mm.
The working spectral range 330,0 — 225,0 nm.
Evaporation of the sample and the excitation spectrum is produced in the arc of a DC power of 15 Andthe duration of exposure 1.5 min; the lower electrode with the sample serves as the anode.
One photographic plate is removed on three of the spectrum from one sample of the sample and each reference sample. On the second photographic plate is removed from the other three spectrum sample sample and each reference sample.
(in edition of Changes N 1, approved. By the decree of Gosstandart of the USSR from
The photographic exhibit within the time specified on the label, record, 20 min washed in running water, rinsed with distilled water and dried.
The paragraph was removed. — Amendment No. 1, approved. By the decree of Gosstandart of the USSR from
4.1.2. To determine the content of zinc, arsenic and cadmium spectra of the analyzed samples comparison pictures of the type of spectrograph ISP-28 through a three-stage attenuator and a width of slit of the spectrograph Illumination of 0.015 mm. slit to produce a three-lens Achromat condenser (first condenser f = 75 mm is not aromatizirovannaya), the intermediate diaphragm is round.
For photography use of the plate type, W, wavelengths 210 to 240 nm.
Evaporation of the sample and the excitation spectrum to produce an arc DC current of 15 A, the exposure time of 45 s, the arc gap of 2.5 mm.
On one disc removed three of the spectrum from one sample of the sample and each reference sample. The plate is treated as described in section
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
On the second photographic plate is removed from the other three spectrum sample sample and each reference sample.
(in edition of Changes N 1, approved. By the decree of Gosstandart of the USSR from
5. PROCESSING OF THE RESULTS
5.1. Fotometrirovanie spectrograms and processing of analysis results
In each spectrogram photometric the blackening of analytical lines of the designated element and the surrounding background to the right and to the left of the analytical lines given in table. 2.
Table 2
──────────────────────────┬───────────────────────────────────────
The designated item │ of the wavelengths of the analytical lines, nm
──────────────────────────┼───────────────────────────────────────
Lead │283,31
Arsenic │234,98
Iron │302,05
Tin │234,00
Silicon │250,69
Zinc │213,86
Bismuth │306,77
Gold │267,59
Nickel │305,08
Copper │327,39
Cadmium │228,80
Magnesium │279,55
Manganese │279,48
Silver │328,07
The average of the two background measurements taken for true darkening .
Calculate the difference .
From the received values are transferred to the corresponding logarithm of relative intensity using the data provided in the application GOST 13637.1−77.
For each of the photographic plates obtained by the values of lg c and sample comparison build for each impurity in the samples of the comparison of the calibration graph in the coordinate and lgc.
Found on each of the spectrograms and the corresponding values to them using the calibration graph, find the content of impurities (one definition).
The result of the analysis is determined as the arithmetic mean of the results of the six definitions from two plates.
In the analysis of antimony brands Su000, Su00, su0, SS1 and SS2 are the calibration graph built in coordinates of logarithm of concentrations of the identified impurities and pochernenija her lines.
Depending on the contents defined impurities photometric appropriate analytical line in the spectrum of the diluted or undiluted sample. The blackening of the selected line should not be less than 0.3 and more than 1.8.
Dilution mass fraction determined by impurities in the sample (X) in percent is calculated by the formula
X = x K,
where With — mass share of impurities in the diluted sample, %;
K — coefficient of dilution.
The difference between the largest and smallest results of six parallel measurements obtained at the two photos at confidence probability P = 0,95, shall not exceed the allowable absolute differences calculated by the formula
where is the arithmetic mean of the six results of parallel measurements obtained on two photographic plates.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
The difference between two results of analysis of the same samples at a confidence probability P = 0.95 does not exceed the allowable absolute differences calculated by the formula
where — the average of the two results of the analysis.
(as amended by Change No. 1, approved. By the decree of Gosstandart of the USSR from
