GOST 9717.1-82

• gost-97171-82.pdf (221.65 KiB)
  ГОСТ 9717.1-82

STATE STANDARDS OF THE USSR

COPPER

METHODS of SPECTRAL analysis GOST 9717.1−82-GOST 9717.3−82

Edition official

Mr.

$

BZ 10-

IPK PUBLISHING house of STANDARDS, Moscow

UDC 669.3:543.42:006.354 Group B59

STATE STANDARD OF THE USSR

copper

Method of spectral analysis on a metal standard samples with photoelectric GOST

peiMcipauMc¹ spectrum 9717.1−82

Copper. Method of spectral analysis of metal standart spccimcns with photoelectrical registration of spectrum

AXTU 1709

Date of introduction 01.07.83

This standard specifies the metl spectral analysis, but the metal standard samples (SS) with photoelectric registration of spectrum copper grades M0k, Ml, M06. Ml, M1 °F. M2r, MWR, M2 and M3 according to GOST 859.

The method is based on the excitation spectrum of the arc discharge AC followed by registration of its optical and quantum Strom.

The method allows to determine the content Prissy p interval mass fraction:

1

1

€> Publishing house of standards, 1982 €> IPK standards Publishing house, 1997 Reprint with Changes

2−1255

C. 2 GOST 9717.1−82

Nickel

Iron

Manganese

Pigs

Chrome

Zinc

phosphorus

0,001 -0.3 0.001 -0.08 0.0003−0.01 0.0005−0.06 0,002 -0,05 0,0008−0,06 0,00! -0.06

The method is characterized by the relative standard deviation Sf single measurement is shown on table. 1. Table I

1.1. General requirements for method of analysis according to GOST 25086. Sampling for analysis according to GOST 546 or GOST 193. (Changed edition, Rev. No. I).

1.2 Mass fraction of elements is determined from two parallel definitions.

1.3. Safety requirements when performing tests according to GOST 27981.0.

1.2. 1.3. (Added, Rev. No. 1).

2

GOST 9717.1−82 S. Z

2. EQUIPMENT AND MATERIALS

Photovoltaic plant (quantometer) Gina DFS-10M, DFS-DFS or 36−56, or MFS-8 or another type.

Generators of the type geu-1, UGE-4, etc.

To register их1учения lines of arsenic (234,98 nm) and lines of comparison (background 228,3 nm) is used photomultipliers type FEU-5, which are mounted without mirrors. For lines of other elements and other lines of comparison, using photomultipliers type FEU-4 and photocells f-1.

Electrodes of copper grades Mob or Ml according to GOST 859 7−8 mm, sharpened to a hemisphere or a truncated cone with ground diameter of 1.5−1.7 mm.

Electrodes made of coal of high purity 6 mm in diameter, sharpened to a hemisphere or truncated cone.

The electrodes are made of copper of the mark Mob or Ml or coal of high purity in the form of bars with diameter 6−7 mm, sharpened to a hemisphere or truncated-, cluded cone with ground diameter of 1.5−1.7 mm.

A device for grinding coal or copper electrodes, for example, the machine model CP-35.

Lathe for sharpening and analyze samples on the plane of the type of TV 16.

Standard samples for composition of copper for spectral analysis.

The analysis used. included in the State register (GSO), and industry (OSO), or standard samples of the enterprise (SOP), approved in the established order. Use standard samples, the sum of mass fractions of certified components which are not different from the sum of the mass fractions of components in the sample more than twice.

Manufactured in the company SOPS for physical and mechanical properties (casting method, processing) should correspond to the analyzed samples.

Allowed to use other equipment, equipment and materials, provided that the metrological characteristics of the analysis, no worse than provided by this standard.

Graphite crucibles.

A muffle furnace with thermostatic control.

3

2'

C. 4 GOST 9717.1−82

The technical rectified ethyl alcohol according to GOST 18300. Consumption of alcohol per one definition in ' 10

Nitric acid according to GOST 4461, diluted 1:10.

Distilled water according to GOST 6709.

(Changed edition, Rev. No. 1).

3. PREPARATION FOR ASSAY

3.1. Sample preparation and analysis must be the same type for each series of measurements. For samples taken n saw a monolithic piece weighing more than 50 g, apply the relevant mass monolithic S. O. Mass of test portions of the sample and should differ no more than twice.

Sample preparation, or conduct a sweep of one of its faces on a plane with a file or cutting tool (the machine) without coolant and lubricant. The stripped surface should be a flat pad with a diameter of not less than 10 mm without holes, scratches, cracks, and slag inclusions. Surface contamination is not allowed.

For samples taken in the form of rods with diameter from 6 to 10 mm, is used in the form of rods with a diameter of 7−8 mm.

Allowed to the pins of the chip, powder, wire, thin sheets, pellets, etc., with a mass less than 50 g by melting at a temperature (1225±25)'in crucibles with an internal diameter of not less than 7 mm and not more than 15 mm, made of spectral pure graphite. The alloy is kept in molten state no more than I min and cooled in a crucible.

Samples and (in the form of rods) are adjusted on the machine in a truncated cone with ground diameter of 1.5−1.7 mm or hemisphere, or on a plane.

Sample and cleaned from surface contamination by etching them in nitric acid (1:1), rinsed with distilled water, rubbed with alcohol and dried.

(Changed edition, Rev. No. 1).

4. ANALYSIS

4.1. The sample or in the form of a monolithic piece is clamped in the lower clamp of the tripod and down the floor a copper or carbon electrode so that the distance from ubeskrivelig plot

4

GOST 9717.1−82 p. 5

to the edge of the sample was not less than the sparking spots (2−5 mm). Allowed the use of samples or in the form of pairs of rods with a diameter of 7−8 mm.

Between the ends of the electrodes are moved apart to (1,50±0,02) mm, ignite the arc to an alternating current power 6−8 And fed with the aid of a standard generator of geu-1 to quantomeno DFS-10M from the mains (220±5) V. Method of controlling the phase with the phase of firing 90*. Pre-firing 10−35 s, the exposure time is not болсс120 C. the Width of the entrance slit of 0.02−0.07 mm. Xel Input light with the aid of a raster condenser. From each sample, WITH and get at least two to three dimensions.

The wavelengths of the analytical lines and lines of comparison are given in table 2 and 3.

Table 2

Table 3

P. 6 GOST 9717.1−82

Continuation of table 3 D SNL full line Attumra determined to"

Allowed the use of other analytical lines and lines of comparison provided that they provide the metrological characteristics of the analysis and the lower boundary of the designated concentrations that meet the requirements of this standard.

(Changed edition, Or*m >b I).

5. PROCESSING OF THE RESULTS

5.1. Throat calibration graphs in the coordinate- !g C or p-C, where the mass fraction of the element in.

p — readings of the output of the measuring device, is proportional to the logarithm of the relative intensity of the lines of the designated element and the comparison lines (background or copper).

The basic method for graphing is a method of «three standards* allowed the use of other methods of graphing method, for example, the solid calibration curve, method of control standard or equation of these curves when processing on a computer.

5.2. Mass fraction of detectable elements in the sample find the calibration schedule on the value of l computed in two (three) dimensions L.

5.3. The analysis result should be the arithmetic mean of two parallel definitions, if the difference

6

GOST 9717.1−82 p. 7

between them at a confidence level P-0.95 does not exceed the value calculated by the formula

rf,-2.77 j? S_r,

where X is the arithmetic mean of two parallel definitions %; S_r — relative standard deviation.

Sang is exceeded, repeat analysis of new navsoc the same sample. In the case of repeated discrepancies analyze a new sample.

5.4. The reproducibility of the results of primary and repeated tests are considered satisfactory if the discrepancy between the results of the two tests does not exceed the value calculated by the for-

5.5. Control of accuracy of analysis results — GOST 25086 standard samples for composition of copper periodically, at least once a quarter.

Sec. 5. (Changed edition, Rev. No. 1).

7

S. 8 GOST 9717.1−82

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy

USSR

DEVELOPERS

A. M. Rytikov, A. A., Nemodruk, M. B. Taubkin. M. I. Burmistrov, I. A. Vorobyev

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards, dated March 24, 1982 No. 1199

3. INSTEAD, GOST 9717.1−75

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. The expiration of snaga resolution of the state standard from 03.11.92 No. 1481

6. PEREEZD\NIE (may 1997) with the Change N? 1, approved in November 1992 (ICS 2−93)