GOST 23687.1-79
GOST 23687.1−79 Ligature odnalezienia. Methods for determination of beryllium (with Change No. 1)
GOST 23687.1−79
Group B59
STATE STANDARD OF THE USSR
LIGATURE ODNALEZIENIA
Methods for determination of beryllium
Alloy of copper-beryllium. Methods of the determination of beryllium
AXTU 1709*
______________
* Introduced advanced Edit. N 1.
Date of introduction 1980−07−01
Resolution of the USSR State Committee on standards of June 6, 1979 N 2050 expiration installed from
________________
* Expiration removed by the resolution of Gosstandart of Russia from
The Change N 1, approved and put into effect by the Decree of the USSR State Committee for standards from
Change No. 1 made by the manufacturer of the database in the text IUS N 12, 1984
This standard specifies photoneutrons examinatory and gravimetric methods for the determination of beryllium (with a mass fraction of beryllium from 4 to 12%).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 23685−79.
2. PHOTONEUTRON METHOD FOR THE DETERMINATION OF BERYLLIUM
2.1.The essence of the method
The method is based on the use of photoneutron reactions 
radiation source is antimony-124.
Quantitative measurement of beryllium perform a relative measurement of the neutron flow of the sample and standard solution, irradiated in the same geometrical conditions.
2.2. Apparatus, materials and reagents
Installation photoneutron for the determination of beryllium consists of a neutron radiometer type RNS-63 with a sensor and update the device-type PSO-2; PP-16.
Sensor (damn.1) is housed in a protective lead sheath 1 neutron counters 5 type SNM-11, surrounded by retarder 2 (organic glass according to GOST 17622−72или paraffin according to GOST 23683−79*), of the loading device 4 with a cylindrical cavity of the cuvette 6; isotopologues with isotope 3.
________________
* On the territory of the Russian Federation GOST 23683−89, hereinafter. — Note the manufacturer’s database.
Damn.1
An operating mode of the radiometer is installed in accordance with the characteristics of the used neutron counters and the requirements of the Assembly and operating instructions approved in the prescribed manner. The level of discrimination is chosen such that the ratio of useful signal obtained in the measurement of a standard solution, the background was the highest.
The source of radiation is antimony-124. Change the source block should be performed under the direction of the radiation monitoring service.
Cuvette made of organic glass according to GOST 17622−72 corresponding to the sensor design (Fig.2). Calibration cuvette for suitability carried out in the following way: in each of the cuvettes carried out repeated measurement (at least 20 times) beryllium-containing solution (5 g/DMof beryllium); fit are considered to be the cell for which the deviation of the measurements (in counts per minute) from the average calculated values of all measurements is not more than 0.1 g/DM
.
Damn.2
The stopwatch according to GOST 5072−79.
Analytical scales ADV-200 GOST 24104−80*.
________________
* On the territory of the Russian Federation GOST 24104−2001, hereinafter. — Note the manufacturer’s database.
Box 8B-OS.
Electric tile according to GOST 14919−83.
The beryllium metal.
Hydrochloric acid by the GOST 3118−77, diluted 1:1.
Nitric acid GOST 4461−77.
Universal indicator paper.
A standard solution containing 5 g/DMof beryllium: beryllium sample weighing 25 g placed in a glass beaker with a capacity of 2000 cm
, moistened with water and dissolved in 1000 cm
of hydrochloric acid first at room temperature and then under heating. The cooled solution was filtered through filter «blue ribbon», is diluted with water to about 4500 cm
. If the pH of the solution is greater than 1.0, adding hydrochloric acid to a pH of 1.0 for universal indicator paper. The volume was adjusted solution with water to 5000 cm
, mixed, 50 cm
of solution placed in the cuvette and tightly closed.
Beryllium standard solution establish a gravimetric method (sec. 3) performing 8−10 definitions of different analysts. A standard solution stored in a room where the temperature is 15−28 °C in places protected from direct sunlight.
(Changed edition, Rev. N 1).
2.3. Analysis
20−30 min before work include the equipment for warm-up. Measure the background noise of the installation. The hitch of the ligature with a mass of 3−5 g was dissolved in 25−30 cmof nitric acid, first at room temperature and then under heating. The cooled solution was transferred to volumetric flask with a capacity of 100 cm
, adjusted to the mark with water and mix. Take 50 cm
of the solution in a cuvette and placed in photoneutron installation. Carry out the measurement of the number of neutrons. During the measurement it is recommended to gain 5−10 thousand pulses. The duration of the measurement is determined by the activity of the source, the content of beryllium in the sample, the sensitivity of the installation and should not exceed 15 min.
Similarly irradiate and measure the number of neutrons in the standard solution. The measurement of a standard solution carried out not less than three times in 6−8 hours
(Changed edition, Rev. N 1).
2.4. Processing of the results
2.4.1. Mass fraction of beryllium (a) percentage calculated by the formula
where ,
is the count rate of neutrons from the sample solution and standard solution minus the background pulse/min;
— the mass of beryllium in 50 cm
standard solution, g;
— the mass of the ligature 50 cm
of the analyzed solution,
(Changed edition, Rev. N 1).
2.4.2. The relative standard deviation is 0.03.
(Changed edition, Rev. N 1).
3. EXAMINATORY GRAVIMETRIC METHOD FOR THE DETERMINATION OF BERYLLIUM
3.1. The essence of the method
Beryllium is precipitated in the form of a complex salt of composition [Co (NH)
]·[Be
O (CO
)
]·X·H
O resulting from the interaction of the carbonate complex of beryllium with cobalt (III) examination. Aluminum, iron, calcium, magnesium and other cations bind in a complex with Trilon B.
3.2. Apparatus, materials and reagents
Desiccator, type EV GOST 25336−82.
Vacuum gauge according to GOST 8625−77.
Filters glass type TF-32 according to GOST 25336−82.
Analytical scales ADV-200 GOST 24104−80.
Hydrochloric acid by the GOST 3118−77, diluted 1:1.
Nitric acid GOST 4461−77 diluted 1:1.
Salt is the disodium Ethylenediamine-N, N, N', N'-tetraoxane acid, 2-water (Trilon B) according to GOST 10652−73, 15% solution: 150 g of salt is poured 500 cmof water, stirred and slurry ammonia is added to dissolve the precipitate (solution pH should be 8−9 on universal indicator paper). The solution was filtered and diluted with water to 1000 cm
.
Ammonia water according to GOST 3760−79.
Ammonium carbonate according to GOST 3770−75, solution, saturated at a temperature of 20−25 °C.
Cobalt (III) esaminare:
saturated solution: 140 g of salt is dissolved in 2000 cmof water heated to a temperature of 70 °C and left for 12 h at room temperature;
a solution with a mass concentration of 2 g/DMwith a pH of 8−9; set pH for universal indicator paper by adding ammonia.
Rectified ethyl alcohol according to GOST 18300−72*.
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* On the territory of the Russian Federation GOST 18300−87. — Note the manufacturer’s database.
The ethyl ether medical. Working with ether in the presence of open flame is prohibited.
Wash solution: 60 cmof ethyl alcohol is diluted to 100 cm
of 0.2% solution of cobalt (III) examinarea and establish a pH of 8−9 at the universal indicator paper by adding ammonia.
Universal indicator paper.
Glassware volumetric laboratory glass according to GOST 1770−74, calibrated.
Electric tile according to GOST 14919−83.
3.3. Analysis
A portion of the ligature mass of 1 g was placed in a beaker with a capacity of 300 cmand dissolved in 20−25 cm
of nitric acid, adding it in small portions. After the cessation of violent reaction solution is heated to boiling, cooled, transferred to a volumetric flask with a capacity of 100 cm
, adjusted to the mark with water and mix.
In a glass with a capacity of 100 cmselect 20 cm
of the initial solution, add 5 cm
Trilon B, is neutralized with ammonia to falling out of beryllium hydroxide, is added 22 mm of ammonium carbonate. The solution is heated on a water bath to a temperature of 40 °C, can withstand up to complete dissolution of the precipitated hydroxide of beryllium, added 3−4 drops of ammonia and precipitated beryllium 12 cm
of a saturated solution of cobalt (III) examinarea, adding it drop by drop from a burette and stirring the solution with a glass rod. After deposition wash the wand with water, washing away with it a precipitate in the same beaker, dilute with water to 100 cm
order water jet to mix the contents of the glass, and stand at least 3−4 hours
Precipitate was filtered under vacuum. Filters previously boiled in hydrochloric acid, washed under vacuum with water, alcohol, ether, prosushivayut air for 15 min and weighed. The precipitate transferred to the filter with a solution with a mass concentration of 2 g/DMcobalt (III) examinarea, wiping the sides and bottom of a glass wand with a rubber tip. Washed precipitate on the filter with 50−60 cm
of this solution, then twice 5 cm
wash solution, 5 cm.
of alcohol, 5 cm
of air. After 2−3 minutes turn off the vacuum, put the filter with the precipitate in a desiccator, the bottom of which is poured water, and kept at a negative pressure 53320−66650 PA (400−500 mm Hg.St.) for 1 h, after which vzvesi
ayut.
3.2, 3.3. (Changed edition, Rev. N 1).
3.4. Processing of the results
3.4.1. Mass fraction of beryllium (a) percentage calculated by the formula
where is the mass of sediment, g;
0,0391 — conversion factor with the complex salts of beryllium on beryllium; — the weight of the portion of the ligature,
3.4.2. The relative standard deviation of analysis results is 0,015.
(Changed edition, Rev. N 1).
3.4.3. Gravimetric method is used when disagreement in assessing the quality of ligatures.
