GOST 851.10-93

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  ГОСТ 851.10-93

GOST 851.10−93 Magnesium primary. Spectral method for determination of silicon, iron, Nickel, aluminum, copper, manganese and titanium

GOST 851.10−93

Group B59

INTERSTATE STANDARD

MAGNESIUM PRIMARY

Spectral method for determination of silicon, iron, Nickel, aluminum,
copper, manganese and titanium

Primary magnesium.
Spectral method for determination of silicon, iron, nickel, aluminium,
copper and manganese

ISS 77.120.20
AXTU 1709

Date of introduction 1997−01−01

Preface

1 DEVELOPED by the Ukrainian scientific-research and design Institute of titanium

INTRODUCED by Gosstandart of Ukraine

2 ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 33 dated February 17, 1993)

The adoption voted:

3 Decree of the Russian Federation Committee on standardization, Metrology and certification from February, 20th, 1996 N 21 inter-state standard GOST 851.10−93 introduced directly as state standard of the Russian Federation from January 1, 1997

4 REPLACE GOST 851.10−87

5 REISSUE

INFORMATION DATA

REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

This standard specifies the spectral method for determination of silicon, iron, Nickel, aluminum, copper, manganese and titanium in the primary magnesium.

The method allows to determine the mass fraction of elements, %:

The method is based on excitation of atoms of magnesium and of the determined elements arc discharge or high voltage spark discharge, the decomposition of the radiation into a spectrum, photographic or photoelectric registration of analytical signals proportional to the intensity or the logarithm of the intensity of spectral lines and subsequent determination of the mass fraction of elements in the sample, using the calibration parameters.

1 General requirements

1.1 General requirements to the method of analysis according to GOST 25086.

1.2 the result of the analysis be the arithmetic mean of results of two parallel measurements.

1.3 To construct the calibration graphs using standard samples. Each point of calibration curve is based on the average result of two parallel measurements.

2 Equipment, reagents and solutions

2.1 General purpose

Universal type generator UGE-4, IVS-28 or similar devices.

Lathe type TV-16 or similar machines.

Trousers shaped with a bending radius of ~ 5 mm.

Set of standard samples with ranges of impurity elements, covering the limits of element contents in the primary magnesium (Mg GSO 5162−5170).

Ethyl alcohol — GOST 18300.

Calico — GOST 29298*.
_______________
* Since 01.01.2007 in the territory of the Russian Federation GOST 29298−2005, here and hereafter. — Note the CODE.

Baptiste — GOST 29298.

Tweezers — GOST 21241.

2.2 With photographic registration of spectrum

The quartz spectrograph medium dispersion type of ISP-30 or similar devices.

Spectromancer type SP-18 or similar devices.

Microphotometer type MF-2 or similar devices.

Photographic plates spectrographic types: AND, ES, UPS, SFC and others.

Developer:

solution a:

distilled water according to GOST 6709 — 1000 cm;

metol (para — methylaminophenol) according to GOST 25664 — 1 g;

sanitarily sodium (sodium sulfite) anhydrous GOST 195 — 26 g;

hydroquinone (paradoxians) according to GOST 19627 — 5 g;

solution B:

distilled water according to GOST 6709 — 1000 cm;

the anhydrous sodium carbonate according to GOST 83 — 20 g;

potassium bromide according to GOST 4160 — 1,

Before the manifestation of the solutions A and b mixed in a volume ratio of 1:1.

Fixer:
distilled water according to GOST 6709 — 1000 cm;

sodium thiosulfate (sodium hyposulfite) according to GOST 244 — 300 g;

sanitarily anhydrous sodium GOST 195 — 26 g.

2.3 allowed the use of developer and fixer of other compositions which do not deteriorate the quality of the photographic registration of the spectrum.

2.4 by the photoelectric registration of spectrum

The installation of a photovoltaic type DFS-36, MFS-8 or similar devices.

3 Preparation for assay

The sample is cast in a two-chetyrehstennoy metal mold with a diameter of 9 mm with tight lock to avoid bays. The cast sample shall be dense, sinks and slag inclusions. Electrodes cut from the sprue, the ends of the electrodes are sharpened on a lathe to the hemisphere. The appearance of shells on a spherical electrode surface, the latter is adjusted until then, until the defect.

4 analysis

4.1 Measurement on the spectrograph produced in the coverage gap are being, or single-lens condenser with fully open intermediate diaphragm.

For the excitation spectrum of atoms of silicon, iron, Nickel, aluminum, copper, manganese and titanium using arc AC discharge parameters: current intensity — (4,0±0,2) A, pre-firing (5±1) s, the exposure time is adjusted depending on the sensitivity of photographic plates, the analytical gap between two identical electrodes (2,0±0,1) mm. the Amount of space measured pattern and the method of shadow projection.

Not allowed aperturing of the light source, emitting clouds arc exposed edges of the samples or frames of parts of the condenser or of a spectrograph.

On one photographic plate photographed in the same conditions as the standard samples and the samples not less than twice.

4.2 For measuring the mass fraction of aluminum, copper, manganese, silicon, iron, Nickel PV installation is used for the excitation spectrum of the arc AC discharge parameters: current intensity — (2,5−4,0) And depending on the sensitivity of the photomultipliers, the voltage supply network — (220±10), the phase of firing is 90°, the repetition frequency of discharges — 100 pulse/s, the discharge inductance is 10 µhz, the discharge resistance of the variable resistor is 1.5 Ohms.

Analytical interval — (2,0±0,1) mm set in the measuring scale of the indicating drum or pattern.

4.3 Measurement of the mass fraction of titanium to produce photovoltaic installation, using the excitation spectrum of the high-voltage spark generator UGE-4 with discharge parameters: voltage — (220±10) V, discharge current — (2,0−4,0) And the scheme is «complex», the value of the subsidiary period of — (3,0±0,1) mm, the capacitance of the capacitor discharge circuit is 0.02 UF, the discharge inductance is 10 µh, the discharge frequency of 300−400 Hz, the analytical gap — (2,0±0,1) mm, without firing the integration time is approximately 90 s, depending on the sensitivity of the photomultiplier.

4.4 it is permitted to use other devices, equipment, materials, modes of excitation and registration of spectral lines under conditions obtaining metrological characteristics meet the requirements of this standard.

5 Processing of analysis results

5.1 Mass fraction of impurities when working in the spectrograph determine fotometriya spectrogram on microphotometer.

As internal standard used the blackening of background.

Use the following wavelengths nm, which corresponds to the analytical lines of impurity elements:

The blackening of analytical lines of the determined elements and background must be in the region of the rectilinear part of the characteristic curve of photographic plates.

In each spectrogram, measure the blackening of analytical lines and calculate the difference of pochernenija analytical lines of the designated impurities and background.

Obtained for each standard sample values for the analytical lines and the background, calculate the average difference pucherani . The calibration graphs are built in coordinates

or

,

where  — mass fraction of silicon, iron, Nickel, aluminum, copper, manganese, titanium, specified in the certificate of standard sample;

 — the average value of the difference pucherani analytical lines and background;

,  — intensity of spectral lines and background for the standard sample.

The abscissa shows the delay value and the y — axis a corresponding amount or

.

In the constructed calibration chart find the mass percent of impurities.

5.2. Mass fraction of impurities when working on the photovoltaic installation is determined by building calibration charts in the coordinates or where the readings of the output of the measuring device.

Use the following wavelengths nm, which corresponds to the analytical lines of the determined elements:

As «internal standard» use line comparison of magnesium 382,99 nm.

5.3 the use of other analytical lines subject to receipt of the metrological characteristics meet the requirements of this standard.

5.4 Standards of accuracy of analysis results

Discrepancies between the results of parallel measurements () and the results of two tests performed in different conditions (a), shall not exceed (at p = 0.95) of the values given in table 1. The error analysis results (at p = 0.95) does not exceed the limit given in table 1.

Table 1

5.5 Control of accuracy of analysis results

5.5.1 the Control of accuracy of analysis results is carried out by comparison with the results of the analysis performed by chemical methods according to GOST 851.1−851.6 GOST; GOST 851.9.

The results of the analysis are believed to be accurate, if the condition

,

where the result of analysis of control samples obtained by the present method;

 — the result of the analysis of the same samples obtained by the chemical method;

, is governed by the standards of the permissible differences between results of the analyses for respectively the spectral and chemical methods.

5.5.2 accuracy Control is carried out before the beginning of the shift or at the same time analysis of batch production samples, but not less than once per month.