By visiting this site, you accept the use of cookies. More about our cookie policy.

GOST 13637.2-93

GOST 33729-2016 GOST 20996.3-2016 GOST 31921-2012 GOST 33730-2016 GOST 12342-2015 GOST 19738-2015 GOST 28595-2015 GOST 28058-2015 GOST 20996.11-2015 GOST 9816.5-2014 GOST 20996.12-2014 GOST 20996.7-2014 GOST P 56306-2014 GOST P 56308-2014 GOST 20996.1-2014 GOST 20996.2-2014 GOST 20996.0-2014 GOST 16273.1-2014 GOST 9816.0-2014 GOST 9816.4-2014 GOST P 56142-2014 STATE STANDARD P 54493-2011 GOST 13498-2010 STATE STANDARD P 54335-2011 GOST 13462-2010 STATE STANDARD P 54313-2011 GOST P 53372-2009 GOST P 53197-2008 GOST P 53196-2008 GOST P 52955-2008 GOST P 50429.9-92 GOST 6836-2002 GOST 6835-2002 GOST 18337-95 GOST 13637.9-93 GOST 13637.8-93 GOST 13637.7-93 GOST 13637.6-93 GOST 13637.5-93 GOST 13637.4-93 GOST 13637.3-93 GOST 13637.2-93 GOST 13637.1-93 GOST 13637.0-93 STATE STANDARD 13099-2006 GOST 13098-2006 GOST 10297-94 GOST 12562.1-82 GOST 12564.2-83 GOST 16321.2-70 GOST 4658-73 GOST 12227.1-76 GOST 16274.0-77 GOST 16274.1-77 GOST 22519.5-77 GOST 22720.4-77 GOST 22519.4-77 GOST 22720.2-77 GOST 22519.6-77 GOST 13462-79 GOST 23862.24-79 GOST 23862.35-79 GOST 23862.15-79 GOST 23862.29-79 GOST 24392-80 GOST 20997.5-81 GOST 24977.1-81 GOST 25278.8-82 GOST 20996.11-82 GOST 25278.5-82 GOST 1367.7-83 GOST 26239.9-84 GOST 26473.1-85 GOST 16273.1-85 GOST 26473.2-85 GOST 26473.6-85 GOST 25278.15-87 GOST 12223.1-76 GOST 12645.7-77 GOST 12645.1-77 GOST 12645.6-77 GOST 22720.3-77 GOST 12645.4-77 GOST 22519.7-77 GOST 22519.2-77 GOST 22519.0-77 GOST 12645.5-77 GOST 22517-77 GOST 12645.2-77 GOST 16274.9-77 GOST 16274.5-77 GOST 22720.0-77 GOST 22519.3-77 GOST 12560.1-78 GOST 12558.1-78 GOST 12561.2-78 GOST 12228.2-78 GOST 18385.4-79 GOST 23862.30-79 GOST 18385.3-79 GOST 23862.6-79 GOST 23862.0-79 GOST 23685-79 GOST 23862.31-79 GOST 23862.18-79 GOST 23862.7-79 GOST 23862.1-79 GOST 23862.20-79 GOST 23862.26-79 GOST 23862.23-79 GOST 23862.33-79 GOST 23862.10-79 GOST 23862.8-79 GOST 23862.2-79 GOST 23862.9-79 GOST 23862.12-79 GOST 23862.13-79 GOST 23862.14-79 GOST 12225-80 GOST 16099-80 GOST 16153-80 GOST 20997.2-81 GOST 20997.3-81 GOST 24977.2-81 GOST 24977.3-81 GOST 20996.4-82 GOST 14338.2-82 GOST 25278.10-82 GOST 20996.7-82 GOST 25278.4-82 GOST 12556.1-82 GOST 14339.1-82 GOST 25278.9-82 GOST 25278.1-82 GOST 20996.9-82 GOST 12554.1-83 GOST 1367.4-83 GOST 12555.1-83 GOST 1367.6-83 GOST 1367.3-83 GOST 1367.9-83 GOST 1367.10-83 GOST 12554.2-83 GOST 26239.4-84 GOST 9816.2-84 GOST 26473.9-85 GOST 26473.0-85 GOST 12645.11-86 GOST 12645.12-86 GOST 8775.3-87 GOST 27973.0-88 GOST 18904.8-89 GOST 18904.6-89 GOST 18385.0-89 GOST 14339.5-91 GOST 14339.3-91 GOST 29103-91 GOST 16321.1-70 GOST 16883.2-71 GOST 16882.1-71 GOST 12223.0-76 GOST 12552.2-77 GOST 12645.3-77 GOST 16274.2-77 GOST 16274.10-77 GOST 12552.1-77 GOST 22720.1-77 GOST 16274.4-77 GOST 16274.7-77 GOST 12228.1-78 GOST 12561.1-78 GOST 12558.2-78 GOST 12224.1-78 GOST 23862.22-79 GOST 23862.21-79 GOST 23687.2-79 GOST 23862.25-79 GOST 23862.19-79 GOST 23862.4-79 GOST 18385.1-79 GOST 23687.1-79 GOST 23862.34-79 GOST 23862.17-79 GOST 23862.27-79 GOST 17614-80 GOST 12340-81 GOST 31291-2005 GOST 20997.1-81 GOST 20997.4-81 GOST 20996.2-82 GOST 12551.2-82 GOST 12559.1-82 GOST 1089-82 GOST 12550.1-82 GOST 20996.5-82 GOST 20996.3-82 GOST 12550.2-82 GOST 20996.8-82 GOST 14338.4-82 GOST 25278.12-82 GOST 25278.11-82 GOST 12551.1-82 GOST 25278.3-82 GOST 20996.6-82 GOST 25278.6-82 GOST 14338.1-82 GOST 14339.4-82 GOST 20996.10-82 GOST 20996.1-82 GOST 12645.9-83 GOST 12563.2-83 GOST 19709.1-83 GOST 1367.11-83 GOST 1367.0-83 GOST 19709.2-83 GOST 12645.0-83 GOST 12555.2-83 GOST 1367.1-83 GOST 9816.3-84 GOST 9816.4-84 GOST 9816.1-84 GOST 9816.0-84 GOST 26468-85 GOST 26473.11-85 GOST 26473.12-85 GOST 26473.5-85 GOST 26473.7-85 GOST 16273.0-85 GOST 26473.3-85 GOST 26473.8-85 GOST 26473.13-85 GOST 25278.13-87 GOST 25278.14-87 GOST 8775.1-87 GOST 25278.17-87 GOST 18904.1-89 GOST 18904.0-89 STATE STANDARD P 51572-2000 GOST 14316-91 GOST P 51704-2001 GOST 16883.1-71 GOST 16882.2-71 GOST 16883.3-71 GOST 8774-75 GOST 12227.0-76 GOST 12797-77 GOST 16274.3-77 GOST 12553.1-77 GOST 12553.2-77 GOST 16274.6-77 GOST 22519.1-77 GOST 16274.8-77 GOST 12560.2-78 GOST 23862.11-79 GOST 23862.36-79 GOST 23862.3-79 GOST 23862.5-79 GOST 18385.2-79 GOST 23862.28-79 GOST 16100-79 GOST 23862.16-79 GOST 23862.32-79 GOST 20997.0-81 GOST 14339.2-82 GOST 12562.2-82 GOST 25278.7-82 GOST 20996.12-82 GOST 12645.8-82 GOST 20996.0-82 GOST 12556.2-82 GOST 25278.2-82 GOST 12564.1-83 GOST 1367.5-83 GOST 25948-83 GOST 1367.8-83 GOST 1367.2-83 GOST 12563.1-83 GOST 9816.5-84 GOST 26473.4-85 GOST 26473.10-85 GOST 12645.10-86 GOST 8775.2-87 GOST 25278.16-87 GOST 8775.0-87 GOST 8775.4-87 GOST 12645.13-87 GOST 27973.3-88 GOST 27973.1-88 GOST 27973.2-88 GOST 18385.6-89 GOST 18385.7-89 GOST 28058-89 GOST 18385.5-89 GOST 10928-90 GOST 14338.3-91 GOST 10298-79 GOST P 51784-2001 GOST 15527-2004 GOST 28595-90 GOST 28353.1-89 GOST 28353.0-89 GOST 28353.2-89 GOST 28353.3-89 STATE STANDARD P 52599-2006

GOST 13637.2−93 Gallium. Atomic-emission method for the determination of cadmium, lead, zinc


GOST 13637.2−93

Group B59


INTERSTATE STANDARD

GALLIUM

Atomic-emission method for the determination of cadmium, lead, zinc

Gallium. Atomic-emission method for the determination of cadmium, lead, zinc


AXTU 1709

Date of introduction 1995−01−01


Preface

1. DEVELOPED by the Interstate technical Committee 104 «of the Semiconductor and rare metals products. Especially pure metals», State Institute of rare metals (Giredmet)

INTRODUCED by Gosstandart of Russia

2. ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 4−93 of 19 October 1993)

The adoption voted:

   
The name of the state
The name of the national authority
standardization
The Republic Of Armenia
Armastajad
The Republic Of Belarus
Belstandart
The Republic Of Kazakhstan
Gosstandart Of The Republic Of Kazakhstan
The Republic Of Moldova
Moldovastandart
Russian Federation
Gosstandart Of Russia
Turkmenistan
Turkmenistanand
The Republic Of Uzbekistan
Standards
Ukraine
Gosstandart Of Ukraine

3. Resolution of the Committee of the Russian Federation for standardization, Metrology and certification from 02.06.94 N 160 inter-state standard GOST 13637.2−93 introduced directly as state standard of the Russian Federation from 01.01.95

4. REPLACE GOST 13637.2−77

INFORMATION DATA


REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced Paragraph number section
GOST 195−77
Sec. 2
GOST 244−76
Sec. 2
GOST 3773−72
Sec. 2
GOST 4160−74
Sec. 2
GOST 10262−73
Sec. 2
GOST 10690−73
Sec. 2
GOST 11120−75
Sec. 2
GOST 13637.0−93
Sec. 1, 2, n.5.5
GOST 13637.1−93
5.1
GOST 13637.3−93
3.2
GOST 18300−87
Sec. 2
GOST 19627−74
Sec. 2
GOST 23463−79
Sec. 2
GOST 24104−88
Sec. 2
GOST 25664−83
Sec. 2



This standard specifies a direct atomic emission method for the determination of mass fractions of impurities in Gaul:

   
cadmium

from 3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаto 3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка%

lead

from 3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаto 3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка%

zinc

from 3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаto 1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка%


The method is based on measuring the intensity of lines of impurity elements in the spectrum obtained during fractional evaporation of impurities from gallium laced with powdered graphite from a channel of a graphite anode in the arc DC.

Impurities in Gaul determined by calibration graphs constructed in the coordinates: logarithm of ratio of intensity of lines of the designated element to the background intensity (ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка), the logarithm of the mass fraction of the element (ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка).

1. GENERAL REQUIREMENTS


General requirements for methods of analysis and safety requirements according to GOST 13637.2.

2. APPARATUS, MATERIALS AND REAGENTS


The diffraction type spectrograph DFS-8 or similar type with the grating 600 gr/mm spectrograph medium dispersion type of ISP-28 or similar type with two-illumination system (condenser lens F-75, 25 mm in diameter).

The arc generator type DG-2 with optional rheostat or similar type adapted to ignite the DC arc high frequency discharge.

Rectifier 250−300, 30−50 A.

Microphotometer type MF-2 or similar type.

Spectromancer of PS-18 or similar type.

Laboratory scales of the 1st class according to GOST 24104*.
_______________
* On the territory of the Russian Federation GOST 24104−2001. — Note the manufacturer’s database.


Libra torsion bar type W to 500 mg or scales of the same type.

Mortar and pestle made of organic glass.

Box of organic glass.

Grinding machine graphite electrodes.

The shaped graphite electrodes for atomic-emission analysis of high purity-7−4, 6 mm in diameter, sharpened to a cone; or graphite electrodes, machined from high purity graphite rods-7−3, 6 mm in diameter, sharpened to a cone, with apex angle 15 degrees and with a platform with a diameter of 1.5 mm at the tip, burnt in the arc of direct current at 15 And during 15 s.

The shaped graphite electrodes for atomic-emission analysis of high purity-7−4, with a diameter of 6 mm, with a channel depth of 6 mm and a diameter of 4 mm; or graphite electrodes of the same size, machined from high purity graphite rods-7−3, burnt in the arc of direct current at 15 And during 15 s.

Cleaning firing is subjected to each pair of electrodes before measurement (electrode, sharpened to a cone — cathode, the electrode with the channel / anode).

Graphite powder of high purity according to GOST 23463.

Gallium metal, clean at the designated impurities, prepared as specified in GOST 13637.0.

Cadmium oxide according to GOST 11120.

Of lead oxide.

Zinc oxide according to GOST 10262.

Records of the photographic type SFC-04 and type SFC-02 size 9x12 cm or equivalent, providing normal blackening of analytical lines and the surrounding background in the spectrum.

The developer consisting of two solutions for photographic plates, type PFS-04.

Solution A:

   
metol (4-methylaminophenol) according to GOST 25664
2 g
sanitarily anhydrous sodium GOST 195
100 g
hydroquinone (paradoxians) according to GOST 19627
9 g
Water

up to 500 cmГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка.


Solution B:

   
potassium carbonate according to GOST 10690
100 g
potassium bromide according to GOST 4160
3 g
water

up to 500 cmГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка.


Before applying the developer mix equal volumes of solutions A and B and add 5% by volume of ethyl alcohol. The time of development should be one and a half times more than the time specified on the package of photographic plates. The temperature of (20±1) °C.

Developer for photographic plates of type SFC-02 prepared according to GOST 13637.1.

Fixer:

   
sodium thiosulfate crystal according to GOST 244
300 g
ammonium chloride according to GOST 3773 20 g
water

to 1000 cmГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка.


Lamp infrared ikz-500 with voltage regulator type RNO 250−0,5, or controller of a similar type.

The technical rectified ethyl alcohol according to GOST 18300, nederevyannyy and double-distilled in quartz apparatus.

State standard samples (GSO) powder graphite SPG-27 PR GEO 2820−83, diluted powder of graphite is two-fold: in a mortar made of organic glass were placed 2 g GSO, add 2 g of powder graphite and carefully grind the mixture with ethanol for 50 min, and then dried under an infrared lamp.

3. PREPARATION FOR ASSAY

3.1. Sample preparation comparison (OS)

3.1.1. Each comparison sample is prepared immediately before the photographing of the spectrum, placing, as specified in clause 4.1, in the channel of the graphite electrode of 10 mg of the sample in comparison to graphite powder (OSGP) according to claim 3.2 and 100 mg of gallium, net-defined impurities. In terms of the method in accordance with the ratio of the masses of miscible substances, mass fraction of impurity in OS (calculated as mass fraction of admixtures in Gaul) is equal to one-tenth of the mass fraction of the impurities in OSGP.

3.2. Sample preparation comparison, graphite powder (OSGP)

Prepare the basic pattern of comparison for powdered graphite (OOGP) containing 1% cadmium, lead and zinc and 97% of carbon based on the content of the metal and carbon in mixtures of metals and carbon, mechanically mixing graphite powder with oxides of the respective metals. For this sample a mass 0,0114 g of cadmium oxide, 0,0108 g of lead oxide, 0,0124 g of zinc oxide and of 0.9700 g of powdered graphite is placed in a mortar made of organic glass and carefully grind the mixture with ethanol for 50 min, and then dried under an infrared lamp.

In order to avoid introducing dirt grinding in a mortar, and drying under a heat lamp are in the box of organic glass.

AOGP also allowed to cook by introducing the designated elements in the form of solutions (see GOST 13637.3).

ОСГП1-ОСГП8 prepare serial dilution OOGP, and then each subsequent sample is powdered graphite.

The mass fraction of each of the designated impurities in ОСГП1-ОСГП8 (based on mass fraction of metals in mixtures of metals and carbon), added to the mixture of sample powder of graphite and diluted sample, mixing for this sample are given in table.1.

Table 1

       
Marking sample The mass fraction of each of the determined impurities, % The mass of test portions, g
    powder
graphite
diluted sample (symbol)
ОСГП1

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

1,800 0,200 (OOGP)
ОСГП2

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

1,400 0,600 (ОСГП1)
ОСГП3

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

1,333 0,667 (ОСГП2)
ОСГП4

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

1,400 0,600 (ОСГП3)
ОСГП5

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

1,333 0,667 (ОСГП4)
ОСГП6

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

1,400 0,600 (ОСГП5)
ОСГП7

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

1,333 0,667 (ОСГП6)
ОСГП8

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

1,400 0,600 (ОСГП7)



Are given in table.1 sample of powdered graphite and diluted sample was placed in a mortar made of organic glass, carefully triturated with ethyl alcohol for 30 min and dried under an infrared lamp. For ОСГП4-ОСГП8 drink alcohol, double distilled in quartz apparatus.

Grinding in a mortar, and drying under a heat lamp are in the box of organic glass.

When determining the zinc from 3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаto 1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка% use ОСГП1-ОСГП4. For other definitions used ОСГП4-ОСГП8. Mass fraction of impurities in the prepared from these samples comparison of OS (in percent, based on the mass percent of impurities in Gaul) are given in table.2.

Table 2

     
Marking sample Marking to take reference sample (OS) The mass fraction of each
of the designated impurities
in the samples comparison (OS), %
ОСГП1
OC1

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

ОСГП2
OC2

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

ОСГП3
ОС3

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

ОСГП4
ОС4

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

ОСГП5
ОС5

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

ОСГП6
ОС6

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

ОСГП7
ОС7

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

ОСГП8
ОС8

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка



References on graphite powder store in tightly closed containers made of organic glass.

4. ANALYSIS

4.1. When recording the spectrum of the sample in the channel of the graphite electrode with a diameter of 4 mm and a depth of 6 mm is placed in series 10 mg of graphite powder and 100 mg of the sample of gallium pieces no larger than 3 mm in diameter (in order to avoid introducing contaminants to the sample of gallium is ground without removing the crystallized plate from a plastic bag).

When taking the spectrum of each reference sample into the channel of the graphite electrode with a diameter of 4 mm and a depth of 6 mm is placed in series 10 mg of the sample in comparison to graphite powder and 100 mg of gallium, determined by the net impurities, with pieces no larger than 3 mm in diameter.

The lower electrode with the sample of gallium (or reference) is an anode, the upper, sharpened to a cone — cathode. Between the electrodes ignite the arc DC power 15 A and the photographing range with exposure 40 s. During the exposure distance between the electrodes is maintained at 3 mm. Spectra in the region of wavelengths of 200−300 nm photographed with the spectrograph of the DFS-8 with a grating of 600 lines/mm operating in the first order, with an intermediate aperture 5 mm, or a spectrograph medium dispersion type of ISP-28, with an intermediate aperture of 5 mm. Width of slit of the spectrograph in both cases 15 microns. In a cassette load a record of type SFC-04 (in the determination of zinc from 3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаto 1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка% of the spectrum photographed on the photographic plates of type SFC-02).

The spectrum of each sample and the spectrum of each of the samples of the comparison register on the photographic plate three times. In addition, on the same plate thrice photographing range of the basics of samples of comparison; for this purpose, the channel of the graphite electrode with a diameter of 4 mm and 6 mm depth each time, place 10 mg of graphite powder and 100 mg of gallium, net-defined impurities.

Exposed photographic exhibit, washed with water, fixed, washed in running water for 15 min and dried.

5. PROCESSING OF THE RESULTS

5.1. In each spectrogram photometric blackening of analytical lines of the designated element ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка(see table.3) and nearby background ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка(minimum blackening near the analytical line of the element on either side, but with the same side in all the spectra taken on one disc) and calculate the difference pucherani ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка.

Table 3

     
The designated element Wavelength of analytical lines, nm
Notes
Cadmium
228,81
-
Lead
283,31  
Zinc
213,86  
Zinc
328,23

Used for the mass fraction of zinc from 3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаto 1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка%



Three parallel values ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка, ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка, ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаobtained three spectrograms taken for each sample, find the arithmetic mean of the results ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка. According to the obtained average values are transferred to corresponding values of the logarithms of relative intensity ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаusing the table provided in Annex GOST 13637.1.

5.2. If the analytical line of the designated element in the spectra of samples basis of comparison is missing, using the values ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаfor the samples comparison (see table.2) and the obtained values ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка, build a calibration curve in the coordinates ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка. Mass fraction of impurities in the sample find the graph value ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаfor the sample.

5.3. Permissible discrepancies in the results of three parallel relations (the ratio of largest to smallest) and two results of the analysis (the ratio of largest to smallest) are shown in table.4.

Table 4

     
Determined by the impurity Mass fraction, %
The permissible divergence
Cadmium

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

3,0
 

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

2,5
 

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

2,5
Lead

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

3,0
 

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

2,5
 

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

2,5
Zinc (213,86 nm)

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

4,0
 

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

3,0
 

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

3,0
Zinc (328,23 nm)

3·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

3,0
 

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

3,0
 

1·10ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка

3,0



Permitted discrepancies for the intermediate mass fraction calculated using linear interpolation.

5.4. If in the spectra of samples basis of comparison, there is a weak line of the element, then the construction of calibration curve in the coordinates ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка, corrected for the mass fraction of the element in the sample comparisons. An amendment is permissible only under the condition that the mass fraction of the element in the sample comparison does not exceed the specified for the method lower limit of the interval defined by the mass fraction. If this condition is not met, it is necessary to choose for the basis of comparison samples a cleaner at the designated impurities of metallic gallium or graphite powder and phased perform a thorough cleaning of the premises, jobs, used equipment, reagents and materials

After receiving the adjusted calibration curve, calculate the mass fraction of impurities in Gaul, as specified in the claims.5.2, 5.3.

5.5. Control of the correctness of the analysis performed according to GOST 13637.0 or in the presence of state standard samples (GSO) powder graphite SPG-27 PR GEO 2820−83, as follows: in channels three graphite electrodes with a diameter of 4 mm and a depth of 6 mm injected with 100 mg of metallic gallium, pure at the designated impurities, and 10 mg diluted GEO.

Analysis of the mixture is carried out simultaneously with the analysis of samples for PP.4 and 5. For each impurity, calculate the ratio of the greater to the lesser of the two quantities as the result of the analysis of the obtained mixture diluted GSO and 0.5 certified value mass fraction of impurities in GSO. The results of the analysis of samples I think is right with confidence probability ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинкаof 0.95, if the ratio is ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка, where ГОСТ 13637.2-93 Галлий. Атомно-эмиссионный метод определения кадмия, свинца, цинка — is regulated in paragraph 5.3, the permissible discrepancy of the two results of the analysis of the sample of gallium, with a mass fraction of impurities is equal to the result of analysis of a mixture of gallium with a dilute GEO.