GOST 9853.24-96

• gost-985324-96.pdf (424.12 KiB)
  ГОСТ 9853.24-96

GOST 9853.24−96 Titan spongy. Spectral method of determination of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum, tin, magnesium and tungsten

GOST 9853.24−96

Group B59

INTERSTATE STANDARD

TITANIUM SPONGE

Spectral method of determination of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum, tin, magnesium and tungsten

Sponge titanium. Spectral method for determination of vanadium, manganese, chrome, copper, zirconium, aluminium, molybdenum, tin, magnesium and tungsten

ISS 77.120*
AXTU 1709
_________________________________
* In the index «National standards», 2008

OKS 77.120, 77.120.50 — note the manufacturer’s database.

Date of introduction 2000−07−01

Preface

1 DEVELOPED by the Interstate technical Committee for standardization MTK 105, Ukrainian research and design Institute of titanium

SUBMITTED to the State Committee of Ukraine for standardization, Metrology and certification

2 ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 9 dated April 12, 1996)

The adoption voted:

3 Resolution of the State Committee of the Russian Federation for standardization and Metrology dated 19 October 1999 No. 353-St inter-state standard GOST 9853.24−96 introduced directly as state standard of the Russian Federation from July 1, 2000.

4 INTRODUCED FOR THE FIRST TIME

1 Scope

This standard specifies the spectral method for determination of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum, tin, magnesium and tungsten sponge (metal) titanium according to GOST 17746.

The method is based on excitation of atoms of titanium and designated elements in the arc discharge or high frequency induction plasma, 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.

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

2 Normative references

The present standard features references to the following standards:

GOST 83−79 Sodium carbonate. Specifications

GOST 195−77 Sodium sanitarily. Specifications

GOST 244−76 Sodium thiosulfate crystal. Specifications

GOST 2789−73 surface Roughness. Parameters and characteristics

GOST 4160−74 Potassium bromide. Specifications

GOST 4328−77 Sodium hydroxide. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 6709−72 distilled Water. Specifications

GOST 9853.7−96 Titan spongy. Method for the determination of aluminium

GOST 9853.11−96 Titan spongy. Method for determination of copper

GOST 9853.12−96 Titan spongy. Method for the determination of zirconium

GOST 9853.13−96 Titan spongy. Method for determination of tin

GOST 9853.14−96 Titan spongy. Method for determination of magnesium

GOST 9853.15−96 Titan spongy. Method for the determination of molybdenum

GOST 9853.16−96 Titan spongy. Method for the determination of tungsten

GOST 9853.18−96 Titan spongy. Method of determination of manganese

GOST 9853.19−96 Titan spongy. Method for the determination of chromium

GOST 9853.20−96 Titan spongy. Method for the determination of vanadium

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 17746−96 spongy Titanium. Specifications

GOST 18300−87 ethyl rectified technical. Specifications

GOST 19627−74 Hydroquinone (paradoxians). Specifications

GOST 21241−89 Tweezers medical. General technical requirements and test methods

GOST 23780−96 spongy Titanium. Methods of sampling and sample preparation

GOST 25086−87 non-ferrous metals and their alloys. General requirements for methods of analysis

GOST 25664−83 Method (4-methylaminophenol sulfate). Specifications

GOST 28498−90 Thermometers liquid-in-glass. General technical requirements. Test methods

GOST 29298−92* cotton and mixed household. General specifications
________________
* On the territory of the Russian Federation GOST 29298−2005, here and hereafter. — Note the manufacturer’s database.

3 General requirements

3.1 General requirements for the method of analysis according to GOST 25086.

3.2 Selection and preparation of samples is carried out according to GOST 23780.

3.3 the result of the analysis taking the arithmetic average of the results of the two definitions.

3.4 To construct the calibration graphs using standard samples. Each point of calibration curve is based on the average of the results of the two measurements.

4 measuring instruments and auxiliary devices

4.1 General purpose

Lathe TV-16 or similar machines.

The lathe.

Set of standard samples ranges of impurity elements, covering the limits of element contents in titanium (like GSO U1−92-Y6−92 on the register of state standard of Ukraine or N 6493−92−6498−92 on the register of Gosstandart of Russia).

Ethanol (ethyl alcohol) rectified technical GOST 18300.

Calico, Batiste GOST 29298.

4.2 excitation spectrum in the arc discharge

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

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

Arc generator AC UGE-4 or IVS-28 or similar devices.

Installation for grinding carbon electrodes.

Tweezers according to GOST 21241.

Spectromancer of PS-18 and MMP-2 or similar devices.

Microphotometer type MF-2 or IPV-460 or similar devices.

Coals spectral brand OS.h. 7−3 or OS.h. 7−4 with a diameter of 6 mm according to the current normative document.

Spectrographic plates of types I, S, UPS, SFC-01, the SFC-02, the SFC-03 according to the current normative document or plates of any type, ensure the normal blackening of analytical lines.

Fotocity or other vessels for processing photographic plates.

Thermometer laboratory according to GOST 28498.

Developer.

Solution A:

— distilled water according to GOST 6709 — up to 1000 cm;

— metol according to GOST 25664 — 1 g;

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

— hydroquinone according to GOST 19627 — 5 g.

Solution B:

— distilled water according to GOST 6709 — up to 1000 cm;

— sodium carbonate (sodium carbonate) anhydrous GOST 83 — 20 g;

— potassium bromide (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 — up to 1000 cm;

— sodium thiosulfate GOST 244 — 300 g;

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

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

4.4 excitation spectrum in a high frequency induction plasma

Plasma spectrometer PS-4 firms BAIRD (Netherlands) or similar devices.

Argon according to GOST 10157.

Hydrochloric acid OS.h. according to GOST 14261, diluted 1:1.

The standard solutions of the determined elements.

Sodium hydroxide according to GOST 4328, solution mass concentration of 200 g/DM.

Nitric acid according to GOST 4461, of 1.49 g/cm.

Indicator paper Congo according the current normative document.

5 preparation for measurement

5.1 excitation spectrum in the arc discharge

For analysis taking the cast samples prepared for mechanical testing.

Effects of arc discharge is subjected to a flat end or lateral surface of the samples and standard samples.

The analyzed surface is carefully treated with a finishing cutter on a lathe with a roughness of the processed surface is not more than 2.5 µm according to GOST 2789, sharp edges removed (chamfer) and wiped with coarse calico moistened with ethanol. On the surface of samples is not allowed sinks, cracks, nonmetallic inclusions and other defects.

Standard samples with a diameter of 20 mm, a length of 50−100 mm are prepared for analysis in the same way as the analyzed samples.

Spectral coal — rods with a diameter of 6 mm, used as protivoelektrodom should be sharpened to a truncated cone with apex angle 60°±3°. The apex of the cone must be cut at the plane perpendicular to the axis of the rod so as to form a platform with a diameter of (1,0±0,1) mm.

5.2 excitation spectrum in a high frequency induction plasma

When determining the mass fraction of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum, tin and magnesium, the hanging sponge (metal) titanium mass 1.0 g is placed in a conical flask with a capacity of 100 cm, 70 cm pouredhydrochloric acid diluted 1:1 and dissolved by heating. The solution was then cooled, transferred to a volumetric flask with a capacity of 100 cmand adjusted to the mark with water.

Preparation of solutions of standard samples of titanium is carried out in the same way as the analyzed samples.

In the case where the contents of the element goes out of range of contents in standard samples as well as in the determination of magnesium in synthetic solutions comparison prepared by the introduction of standard solutions of the identified elements in a solution of titanium of high purity (the content of vanadium, manganese, chromium, copper, zirconium, aluminum, molybdenum, tin, and magnesium — not more than lower limit of determination by this method), prepared in the same way as the solutions of the analyzed samples.

In the determination of tungsten in titanium solution add 3−4 drops of nitric acid, it is evaporated to 40 cmand neutralize the Congo paper with sodium hydroxide solution the mass concentration of 200 g/DMbefore the dyeing of paper of the Congo from purple to red. Then add 20 cmof the sodium hydroxide solution in excess.

The resulting solution was boiled for 5 min, transferred to a volumetric flask with a capacity of 200 cmand was adjusted to the mark with water. The solution was then filtered through a filter of medium density. The filtrate is used for determining tungsten.

Synthesized solutions comparison for the determination of tungsten is prepared by dilution of a standard solution of tungsten mass concentration of 1 g/DMof distilled water.

6 procedures for measuring

6.1 in the excitation spectrum in the arc discharge

6.1.1 With photographic registration of spectrum

The measurements, the spectrograph was carried out at the illumination slit being or single-lens condenser with fully open intermediate diaphragm. For the excitation spectrum of titanium atoms and atoms of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum and tin using arc AC discharge parameters: current — 6,0−10,0 A, pre-firing (10±1) s, the exposure time is adjusted depending on the sensitivity of photographic plates so that the blackening of analytical lines were in the linear part of the characteristic curve of photographic plates.

The analytical gap is the distance between the surface sample and coal cone of the counter — must be 1,5−2,0 mm Gap measured pattern by the method of shadow projection or on the measuring scale of the indicating drum.

Not allowed aperturing of the light source protruding edges of the sample, rims of the parts of the condenser or of a spectrograph.

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

6.1.2 by the photoelectric registration of spectrum

The measurements were carried out using the excitation spectrum of titanium atoms and atoms of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum and tin arc AC discharge parameters: current — a 4.0 a 6.0 a; voltage — (220±10); the phase of firing is 90°; repetition frequency discharges — 100 imp/s; bit inductance — 10 uh; the firing — 0; exposure time is 50 s.

Analytical in the interelectrode gap of 1.5−2.0 mm is set on the measuring scale of the indicating drum or pattern.

6.2 excitation spectrum in a high frequency induction plasma

Measurements on the plasma spectrometer is carried out under the following conditions of excitation and registration of the spectrum: the generator output to 1.2−1.3 kW; the integration time is 3 s; number of integration, 5; height of observation above the rim of the quartz burner is 16 mm; the feed rate of the sample peristaltic pump — 4 cm/min; the pressure of argon carrying the aerosol — 235 kPa; argon flow, DM/min

transporting the aerosol — 1,1,

plasma — 1,1,

cooling is 13.0.

6.3 permitted the use of other devices, equipment, materials, modes of generating and recording the spectrum under condition of achievement of the metrological characteristics meet the requirements of this standard.

7 Processing measurement results

7.1 Mass fraction of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum and tin when working on the define spectrograph, spectrogram fotometriya on microphotometer.

As internal standard used the line of titanium or background near the line.

Use analytical lines of the elements specified in table 1.


Table 1

In each spectrogram, measure the blackening of analytical pairs of spectral lines and calculate the difference of pochernenija analytical lines of the designated element and the comparison lines (or background).

Obtained for each standard sample values is calculated the average difference pucherani .

The calibration graphs are built in coordinates , where  — mass fraction of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum and tin, specified in the passport on the standard sample;  — the average value of the difference pucherani analytical lines and the comparison lines (or background).

The abscissa shows the delay values and the y — axis corresponding values .

In the constructed calibration chart find the mass percent of the designated element

s.

7.2 Mass fraction of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum and tin at work on a photovoltaic installation with excitation spectrum in the arc discharge determined by building calibration charts in the coordinates or where the readings of the output of the measuring device.

Use the following analytical lines of elements (wavelength, nm):

As internal standard used the line titanium 294,83 nm.

7.3 Mass fraction of vanadium, manganese, chromium, copper, zirconium, aluminium, molybdenum, tin, magnesium and tungsten when working on the plasma spectrometer is determined by building calibration graphs in the coordinate

, (1)

where  — the average value of the intensity of the analytical lines in the comparison solution or in the solution of a standard sample;

 — the intensity of the analytical lines in the solution of titanium of high purity (the content of the analyzed element is not more than the lower limit of determination).

Use the following analytical lines of elements (wavelength, nm):

7.4 the use of other analytical lines and coordinate systems subject to obtaining the metrological characteristics meet the requirements of this standard.

8 Allowable measurement uncertainty

8.1 the difference between the two measurements and the results of two tests performed in different conditions, should not exceed (with confidence probability of 0.95) of the values given in table 2. The error analysis results (at a confidence probability of 0.95) does not exceed the limit given in table 2.


Table 2

Percentage

8.2 Periodic monitoring of the accuracy of the results of spectral analysis carried out by comparing the obtained results with the results of the analysis performed by chemical methods according to GOST 9853.7, 9853.11 GOST-GOST 9853.16, 9853.18 GOST-GOST 9853.20, but not less than once per quarter.

The number of results of spectral analysis, controlled by chemical analysis, establish depending on the total number of incoming samples, but not less than 0.1% of all samples of commercial products coming into the lab for the quarter.

The accuracy of the analysis results shall be considered satisfactory if not less than 95% of cases the condition

, (2)

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;

and  — the permissible discrepancy between the results of the analysis respectively for the spectral and chemical methods.

8.3 Operational control of the accuracy is carried out before the beginning of the shift or at the same time analysis of batch production samples.

For control purposes, choose the standard two sample values of the mass fraction of the element located in the lower and upper limits of the measurement range, and perform measurements of the content of this element in each standard sample. If at least one standard sample analysis result at the operational control differs from the value of the mass fraction of the element at a given point of the calibration characteristics more than 0.5adjust the calibration characteristics.

9 qualifications

To perform analysis allowed spectroscopist qualification not less than 4th category, having II qualifying group with electrical.