GOST 1293.14-83
GOST 1293.14−83 lead-antimony Alloys. Spectral method of determination of sodium, calcium and magnesium (with Amendments No. 1, 2)
GOST 1293.14−83
Group B59
INTERSTATE STANDARD
LEAD-ANTIMONY ALLOYS
Spectral method of determination of sodium, calcium and magnesium
Antimonous lead alloys.
Spectral method for determination of sodium, calcium and magnesium
AXTU 1709
Date of introduction 1985−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
DEVELOPERS
V. P. Savraev, L. K. Larin, N. F. Sachkov (head), V. K. Isupov
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from
3. INTRODUCED FOR THE FIRST TIME
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
The number of the paragraph, subparagraph, enumeration, application |
| GOST 1292−81 |
1.1, 3 |
| GOST 1293.6−78 |
6.3 |
| GOST 1293.8−78 |
6.3 |
| GOST 1293.9−78 |
6.3 |
| GOST 4233−77 |
3 |
| GOST 4526−75 |
3 |
| GOST 4530−76 |
3 |
| GOST 6709−72 |
1.2 |
| GOST 11125−84 |
3 |
| GOST 13348−74 |
2, 3 |
| GOST 14262−78 |
3 |
| GOST 14919−83 |
3 |
| GOST 23463−79 |
3 |
| GOST 24231−80 |
1.1 |
5. Limitation of actions taken by Protocol No. 4−93 of the Interstate Council for standardization, Metrology and certification (ICS 4−94)
6. REPRINT (October 1999) with amendment No. 1, approved in June 1989 (IUS 10−89)
The Change No. 2 adopted by the Interstate Council for standardization, Metrology and certification (Protocol No. 8, dated 12.10.95). The state developer of Kazakhstan. By the resolution of Gosstandart of Russia
Change No. 2 made by the manufacturer of the database in the text ICS N 7, 2001
This standard establishes a spectral method for the determination of sodium, calcium and magnesium in lead-antimony alloys in the range of mass fraction from 0.001 to 0.04%.
The method is based on converting lead-antimony alloy in sulfuric acid salt and subsequent determination of the impurities in the arc mode by the method of «three standards» for the calibration graphs constructed in the coordinates 
(Changed edition, Rev. N 1).
1. GENERAL REQUIREMENTS
1.1. Sampling and preparation for analysis — according to GOST and GOST 1292 24231.
1.2. For analysis and preparation of solutions used additionally distilled in a quartz apparatus, the freshly prepared distilled water according to GOST 6709.
(Changed edition, Rev. N 1).
1.3. A portion of the alloy is transferred into solution in Teflon or quartz containers.
1.4. Control of correctness of the analysis carried out according to GOST 25086−87 by a method of additives or by comparing the results of the analysis of the same samples obtained by this method, with the results of atomic absorption analysis, obtained according to GOST 1293.6−78, GOST 1293.8−78, GOST 1293.9−78 or other certified method every time when replacing the reagents, standard solutions, specimens, comparison, equipment repairs and other changes that affect the result of the analysis.
When using the addition method sample analysis I believe is correct if the found value differs from the additive introduced its value of not more than
where and
— the permissible discrepancy of the results of analysis for sample (
) and samples with the additive (
).
When monitoring the correct implementation of the analysis a comparison of the results of analysis by this method with the results of the analysis of the same samples obtained by an independent test method, samples believe is correct if the difference between the analyses is not more than
where and
— the permissible discrepancy of the two results of the analysis, the numerical value of which is regulated in check (
) and check (
) methods of analysis.
(Changed edition, Rev. N 2).
2. SAFETY REQUIREMENTS
Safety requirements — according to GOST 13348.
3. APPARATUS, MATERIALS AND REAGENTS
The quartz spectrograph medium dispersion type of ISP-30 and the diffraction-type DFS-8 with three-lens Achromat illumination system of the slit and the three-step attenuator.
Allowed the use of other types of spectrographs, subject to obtaining the required sensitivity and metrological characteristics are not worse than specified in item 6.2.
Arc generator of the type PS-39 and IVS-28.
A constant current source.
Microphotometer of any type, intended for measuring the density of blackening of spectral lines.
Libra torsion bar type W with a weighing error of no more than 0.001 g.
Mortar made of organic glass or steel with a pestle.
Electric tile according to GOST 14919.
Cookware PTFE or quartz (cups, glasses, lids).
Nitric acid of high purity according to GOST 11125 and a solution of 1:3.
The graphite powder of high purity according to GOST 23463.
Electrodes, carbon, high purity or-3 6 mm in diameter, with the crater size, 4x4 and 4x8 mm Contractrate coal, sharpened to a truncated cone with ground diameter of 1.5−2 mm.
Photographic plates spectrographic types «panchrom», SFC-02, the SFC-03, NT-2SV at THAT 6−43−1475−88 or other types, allowing to obtain the desired sensitivity of the determined elements.
The developer of photographic plates according to GOST 13348.
Alloy lead-antimony GOST 1292 brands Ssua or a MUSTACHE with a mass fraction of sodium, calcium and magnesium less of 0.0005%.
Sodium chloride according to GOST 4233, h. e. a., dried in a drying Cabinet for 1 h at 100 °C.
Calcium carbonate according to GOST 4530, h. e. a., dried in a drying Cabinet for 1 h at 100 °C.
Magnesium oxide according to GOST 4526, h. e. a., calcined in a muffle for 1 h at a temperature of 600 °C.
Standard solutions.
Solution a: 0,254 g of sodium chloride dissolved in water and transferred to volumetric flask with a capacity of 100 cm.
1 cmof the solution contains 1 mg of sodium.
Solution B: 0,250 g of calcium carbonate dissolved in 100 cmof nitric acid, transferred into a volumetric flask with a capacity of 100 cm
and adjusted to the mark with water.
1 cmof the solution contains 1 mg of calcium.
Solution: 0,166 g of magnesium oxide are dissolved in 10 cmof nitric acid when heated, transferred to a volumetric flask with a capacity of 100 cm
and adjusted to the mark with water.
1 cmof the solution contains 1 mg of magnesium.
Sulfuric acid of high purity according to GOST 14262.
Muffle furnace with temperature up to 600 °C.
Apparatus quartz distillation water.
(Changed edition, Rev. N 1, 2).
4. PREPARATION FOR ASSAY
4.1. For the preparation of the first reference sample a small number (~12−15 g) lead-antimony alloy in the form of chopped pieces or shavings placed in a quartz or Teflon Cup, poured a solution of nitric acid and washed for 30 s. the acid Solution is poured, the alloy was washed with distilled water. From the thus-prepared alloy take weighed 10 g and dissolved in quartz or fluoropolymer Cup in the 70−80 cmof the solution of nitric acid under heating. After complete dissolution, add 4 cm
of the solutions A, B and C and precipitated lead sulfate gradually add 5−7 cm
of sulfuric acid. The solution is carefully evaporated, the precipitate is dried, calcined in a muffle furnace at 500 °C for 1 h.
The resulting reference sample containing 0.04% calcium, magnesium and sodium, based on alloy is ground in a mortar.
The following samples and comparison prepared by subsequent dilution of each newly prepared with a basis in two or two and a half times.
References, containing 0.04; 0,02; 0,01; 0,005; 0,001 and 0,002% for each of the determined impurities, is stored in buksh or other tightly sealed container.
4.2. For cooking basics 30−50 g of lead-antimony alloy is washed, transferred into solution is precipitated in the form of sulphate, is evaporated and calcined, as described in Chapter 4.1. The resulting basis is ground in a mortar and stored in a tightly sealed container.
4.3. Each of the prepared samples are mixed with graphite powder in a ratio of 1:1 (by weight). The samples of the comparison is stored in tightly sealed jars made of polyethylene.
4.1−4.3. (Changed edition, Rev. N 1).
5. ANALYSIS
5.1. Weighed samples of lead-antimony alloy with a mass of 1−2 g was placed in a quartz or Teflon Cup, pour 20−25 cmof a solution of nitric acid, is dissolved, is precipitated in the form of sulphate, is evaporated and calcined, as described in section 4.1. The obtained salt is ground in a mortar, mixed with powdered graphite at a ratio of 1:1 and fill in the crater of a carbon electrode. Upper and lower carbon electrodes are pre-fired in an arc alternating current power of 10 A for 10 s.
Simultaneously conduct control experience for an amendment in the result analysis. For it take 1−2 g of lead-antimony alloy, used for cooking basics, transferred to salt, and photographed simultaneously with the analyzed samples.
To obtain the result of analysis from each sample is taken at the two sample and photographic plate is photographed on three of the spectrum from each of the samples and comparison of six spectra from each sample (three of the spectrum from the sample).
5.2. In the determination of calcium, sodium, magnesium from samples comparison of samples taken sample weighing 30 mg was placed in craters of the carbon electrodes with a size of 4x4 mm for the determination of calcium, magnesium and 4x8 mm in the determination of sodium and burn in the arc of a DC power of 15 A. the exposure Time for the calcium, magnesium 100, sodium — 60 s. the distance between the electrodes 3 mm.
Determination of calcium and magnesium is carried out on the quartz spectrograph of the ISP-30 being the illumination system of the slit. On the slit of the instrument, establish a three-tier reliever. The slot width 0,013 mm.
The determination of sodium is performed on the spectrograph DFS-8 with three-lens Achromat illumination system of the slit. The slot width of 0.01 mm.
The spectra are photographed on photographic plates spectrographic type SFC-02 in the determination of magnesium and «pangram» in the determination of calcium and sodium.
5.1, 5.2. (Changed edition, Rev. N 1, 2).
5.3. To construct the calibration graphs using the following pairs of lines, nm:
magnesium 279,5 — lead 311,8
calcium 393,3 or 396,8 — background
sodium 588,9 — lead 500,5.
(Changed edition, Rev. N 1).
6. PROCESSING OF THE RESULTS
6.1. Spectra of the analyzed samples and comparison samples photographed on the same plate by six and three times respectively. The blackening of analytical lines () and compare (
) are measured on microphotometer. The calibration graphs are built in coordinates
is the average of the three values
— known mass fraction determined by impurities in the samples of the comparison in percent.
According to the obtained values from the graphs determine the mass fraction of impurities in the analyzed samples. When determining a calcium measure the blackening of analytical lines (
). Calibration curve constructed in the coordinates
is the mean value
according to the schedule determine the mass percent of calcium in the analyzed
samples.
6.2. The final result of the analysis be the arithmetic mean of results of two parallel measurements obtained on a single photographic plate, each of the three spectrograms. Discrepancies in the results of parallel measurements (a measure of repeatability) at a confidence probability
of 0.95 does not exceed the values calculated according to the formula
where is the relative standard deviation results of parallel measurements to be equal to the sodium — 0,09; calcium — 0,08; magnesium — 0,06;
— the arithmetic mean of the results of two parallel determinations;
0.95 and
2.
Or
The discrepancy of the two results of the analysis of the same sample (a measure of reproducibility) at a confidence probability
of 0.95 does not exceed the values calculated according to the formula
where is the relative standard deviation of the two results of the analysis of the same sample, equal to sodium — 0,1; calcium — 0,09; for magnesium — 0,06;
— the average of the two results of the analysis, %.
Or
6.1, 6.2. (Changed edition, Rev. N 2).
6.3. The differences in the assessment of quality to determine the use of sodium flame photometric method according to GOST 1293.6; for the determination of calcium — atomic absorption method GOST 1293.8 for determination of magnesium — atomic absorption method GOST 1293.9.
