GOST 23862.5-79

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  ГОСТ 23862.5-79

GOST 23862.5−79 Lanthanum, cerium, europium, gadolinium, lutecium, yttrium and their oxides. Spectral method of determination of vanadium, iron, calcium, cobalt, silicon, magnesium, manganese, copper, Nickel, lead, titanium, chromium, zinc and zirconium (with Amendments No. 1, 2)

GOST 23862.5−79

Group B59

INTERSTATE STANDARD

LANTHANUM, CERIUM, EUROPIUM, GADOLINIUM, LUTECIUM, YTTRIUM AND THEIR OXIDES

Spectral method of determination of vanadium, iron, calcium, cobalt, silicon, magnesium, manganese, copper, Nickel, lead, titanium, chromium, zinc and zirconium

Lanthanum, cerium, europium, gadolinium, lutecium, yttrium and their oxides. Spectral method of determination of vanadium, iron, calcium, cobalt, silicon, magnesium, manganese, copper, nickel, lead, titanium, chromium, zinc and zirconium

ISS 77.120.99
AXTU 1709

Date of introduction 1981−01−01

The decision of the State Committee USSR on standards on October 19, 1979 N 3988 date of introduction is established 01.01.81

Limitation of actions taken by Protocol No. 7−95 Interstate Council for standardization, Metrology and certification (ICS 11−95)

EDITION with Amendments No. 1, 2 approved in April 1985, may 1990 (IUS 7−85, 8−90).


This standard establishes a spectral method for the determination of impurities of vanadium, iron, calcium, cobalt, silicon, magnesium, manganese, copper, Nickel, lead, titanium, chromium, zinc and zirconium in Lantana, of a thermodynamic equilibrium, europium, gadolinium, of Lutetia, yttria (previously translated into oxide) and their oxides.

The method is based on excitation and photographic registration of arc emission spectra of analyzed materials and samples the comparison with the subsequent determination of mass fractions of impurities in the calibration schedule.

Intervals determined by a mass fraction of impurities:

(Changed edition, Rev. N 1, 2).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 23862.0−79.

2. APPARATUS, MATERIALS AND REAGENTS

The diffraction spectrograph DFS-13 with a grating 1200 lines/mm, operating in first order of reflection from being a lighting system or similar.

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

Rectifier 250−300, 30−50 A.

Microphotometer geregistreerde type MF-2 or similar.

Spectromancer PS-18 or similar.

Libra torsion type VT-500 or similar.

Box of organic glass.

Mortars and pestles made of organic glass.

A muffle furnace with a thermostat that provides temperature to 1200 °C.

Drying oven with thermostat providing temperatures up to 120 °C.

Tile electric.

Infrared lamp Z-s-1.

The machine tool for sharpening of electrodes.

Coals spectral high purity-7−3, with a diameter of 6 mm.

The electrodes are machined from high purity coals spectral-7−3, with a diameter of 6 mm:

— type «glass» with a leg diameter 2 mm, height 2 mm, with a crater: with a diameter of 4 mm, depth 3 mm, a height of the outer wall is 4 mm (I); a depth of 5 mm, a height of the outer wall 6 mm (II); a depth of 4 mm, a wall thickness of 1 mm (III); with a diameter of 4.5 mm, a depth of 6 mm, a wall thickness of 1 mm (IV);

— crater with a diameter of 4 mm:

a depth of 4 mm, a wall thickness of 1 mm (V);

a depth of 7 mm, wall thickness 0,5−0,7 mm, a height of the sharpened part 10 mm (VI);

— crater with a diameter of 2 mm:

depth of 5 mm, wall thickness 0,5−0,7 mm, a height of the sharpened part is 8 mm (VII);

depth of 5 mm, a wall thickness of 1 mm (VIII);

with a depth of 3 mm, a wall thickness of 1 mm (IX);

— sharpened to a truncated cone with an apex angle of 15° with the site and the 1.5 mm (X).

Cleaning firing in the arc of direct current at 15 And during 15 put each pair of electrodes directly before analysis.

Graphite powder of high purity according to GOST 23463−79.

Spectrographic plates of the type II or the same size 9х24 or 9x12 for normal blackening of analytical lines and the background in the spectrum.

The quartz Cup with a capacity of 200 cm.

Cup platinum.

The platinum crucibles.

Oxalic acid OS.h. 3−4, a saturated solution.

Nitric acid of high purity according to GOST 11125−84 diluted 1:1 and 1% probability.

Sulfuric acid GOST 4204−77, H. h., diluted 1:1 and 1% probability.

Hydrogen peroxide according to GOST 10929−76.

The technical rectified ethyl alcohol GOST 18300−87, double-distilled in quartz apparatus.

Sodium chloride OS.h. 6−4.

Sodium carbonate according to GOST 83−79.

Calcium oxide according to GOST 8677−76, h.d. a.

Silicon dioxide according to GOST 9428−73, h.d. a.

Magnesium oxide according to GOST 4526−75.

Lead.

Zinc GOST 3640−94.

Zirconium dioxide, H. h

Sulfur, h.d. a.

Silver chloride, H. h

Vanadium.

Radio engineering carbonyl iron brand PS according to GOST 13610−79.

Cobalt grade K-1 or higher according to GOST 123−98*.
________________
* On the territory of the Russian Federation from 01.07.2009 valid GOST 123−2008. — Note the manufacturer’s database.

Manganese metal brands Мр0 or Мр00 according to GOST 6008−90.

Copper grade M3 or higher according to GOST 859−2001.

Nickel, H grade 2 or higher according to GOST 849−97.
________________
* On the territory of the Russian Federation from 01.07.2009 standards 849−2008. — Note the manufacturer’s database.

Titanium.

Chrome brand X00 GOST 5905−79*.
_______________
* On the territory of the Russian Federation GOST 5905−2004. — Note the manufacturer’s database.

Gallium brand GL-1 according to GOST 12797−77.

Oxide of lanthanum, cerium, europium, gadolinium, lutetium, yttrium, clean-defined impurities.

Replacement solutions containing 1 mg/cmvanadium, iron, calcium, cobalt, magnesium, manganese, copper, Nickel, lead and zinc: 100 mg of one of the metals is placed in a beaker and dissolved in 10 cmof nitric acid, diluted 1:1, transferred into a volumetric flask with a capacity of 100 cm, adjusted to the mark with water and mix.

Replacement solutions containing 1 mg/cmof titanium and chromium, 100 mg of corresponding metal dissolved in 20 cmof sulphuric acid diluted 1:1, transferred into a volumetric flask with a capacity of 100 cm, adjusted to the mark with water and mix.

A solution of L containing 0.1 mg/cmof the respective metals, prepared before use: in a volumetric flask with a capacity of 100 cmwith a pipette measure out 10 cmof each of the replacement solutions of vanadium, iron, calcium, cobalt, magnesium, manganese, copper, Nickel, lead and zinc, adjusted to the mark with 1%-s ' solution of nitric acid and stirred.

Solution L1 containing 0.01 mg/cmvanadium, iron, calcium, cobalt, magnesium, manganese, copper, Nickel, lead and zinc, prepared before use by dilution of a solution of L to 10 times 1% nitric acid solution.

The TSE solution containing 0.1 mg/cmof the respective metals, prepared before use: in a volumetric flask with a capacity of 100 cmwith a pipette measure out 10 cmof each of the replacement solutions of iron, calcium, cobalt, magnesium, manganese, copper, Nickel, lead and zinc, adjusted to the mark with 1%-s ' solution of nitric acid and stirred.

Solution C1 containing 0.01 mg/cmiron, calcium, cobalt, magnesium, manganese, copper, Nickel, lead and zinc, prepared before use by diluting the solution TSE 10 times 1% nitric acid solution.

The alternate solution containing 1 mg/cmof silicon: 214 mg of silicon dioxide is placed in a platinum crucible, add 3 g of sodium carbonate and fused in a muffle furnace at a temperature of 1200 °C. After cooling, the crucible was placed in a platinum Cup (pre-wash the bottom of the crucible), add 50−60 cmof water, heated until complete dissolution, transferred to a volumetric flask with a capacity of 100 cm, adjusted to the mark with water, quickly mixed and poured into a polyethylene jar.

LIU solution containing 0.1 mg/cmof cobalt, manganese, copper and Nickel prepared before use: in a volumetric flask with a capacity of 100 cmwas injected by pipette at 10 cmreplacement solutions of these metals, bring to mark 1% nitric acid solution and stirred.

Solution E containing 0.1 mg/cmof iron and copper, prepared before use: in a volumetric flask with a capacity of 100 cmwas injected by pipette at 10 cmreplacement solutions of these metals, bring to mark with a solution of nitric acid with a mass fraction of 1% and stirred.

Solution And containing 0.1 mg/cmof magnesium and lead, prepare before use: in a volumetric flask with a capacity of 100 cmwas injected by pipette at 10 cmreplacement solutions of these metals, bring to mark with a solution of nitric acid with a mass fraction of 1% and stirred.

A solution containing 0.1 mg/cmvanadium, prepared before use by diluting a backup solution vanadium 10 times 1% nitric acid solution.

A solutioncontaining 0.01 mg/cmvanadium, prepared before use by diluting the solution 10 times In 1% nitric acid solution.

The solution M containing 0.1 mg/cmcopper, prepared before use by dilution of a spare copper solution 10 times 1% nitric acid solution.

The solution Mcontaining 0.01 mg/cmcopper, prepared before use by dilution of the solution M is 10 times 1% nitric acid solution.

The solution Mcontaining 0.001 mg/cmcopper, prepared before use by dilution of the solution Mis 10 times 1% nitric acid solution.

Solution T containing 0.1 mg/cmtitanium, prepared before use by diluting a backup solution titanium is 10 times 1% sulfuric acid solution.

Solution Tcontaining 0.01 mg/cmtitanium, prepared before use by dilution of a solution of T 10 times 1% sulfuric acid solution.

Solution X, containing 0.1 mg/cmchromium, prepared before use by diluting a backup solution of chromium in 10 times a 1% solution of sulfuric acid.

Solution Xcontaining 0.01 mg/cmchromium, prepared before use by dilution of a solution X is 10 times 1% sulfuric acid solution.

Solution Xcontaining 0.001 mg/cmchromium, prepared before use by dilution of a solution Xis 10 times 1% sulfuric acid solution.

Ka solution containing 0.1 mg/cmof Sa, prepared before use by diluting a backup solution 10 times with a solution of nitric acid with a mass fraction of 1%.

Ка1 solution containing 0.01 mg/cmof Sa, prepared before use by dilution of a solution of CA 10 times with a solution of nitric acid with a mass fraction of 1%.

To a solution containing 0.1 mg/cm, is prepared before use by diluting a backup solution With 10 times the nitric acid solution with a mass fraction of 1%.

A solution 1 containing 0.01 mg/cm, is prepared before use by diluting the solution To 10 times with a solution of nitric acid with a mass fraction of 1%.

Ко2 solution containing 0.001 mg/cm, is prepared before use by dilution of a solution 1 in 10 times with a solution of nitric acid with a mass fraction of 1%.

Sec. 2. (Changed edition, Rev. N 1, 2).

3. PREPARATION FOR ASSAY

3.1. Preparation of the buffer mixture

3.1.1. In the determination of the oxides of lanthanum impurities of vanadium, iron, cobalt, manganese, copper, Nickel, titanium and chromium buffer mixture, which is a graphite powder containing 2% of gallium oxide, is prepared as follows. In a glass with a capacity of 100 cmplaced 1.5 g of gallium metal, poured 80 cmof nitric acid, diluted 1:1, heated on a heating plate until complete dissolution and is evaporated to a volume of 15−20 cm.

In a quartz Cup was placed 98 g of graphite powder, pour the obtained solution of gallium, add water until mushy state, mixed and dried under a heat lamp for 5−6 h. the resulting mixture was placed in a mortar made of organic glass pestle and stirred for 4 h, periodically adding alcohol, maintaining the mixture in a pasty condition. The mixture was transferred to a quartz Cup and dried in an oven at 90−100 °C for 2−3 h. the Dried mixture was stirred in a mortar for 30 min.

3.1.2. In the determination of dioxide of cerium impurities of iron, cobalt, manganese, copper and Nickel buffer mixture, which is a graphite powder containing 10% of sodium chloride, is prepared by trituration 90 g of powder of graphite and 10 g of sodium chloride in a mortar made of organic glass for 1 h.

(Changed edition, Rev. N 1, 2).

3.1.3. In determining the oxide of europium impurities silicon, iron, copper and zinc buffer mixture, which is a graphite powder containing 2% of sulphur, is prepared by trituration 98 g of graphite powder with 2 g of sulfur in a mortar made of organic glass for 1.5−2 hours.

(Added, Rev. N 2).

3.2. Sample preparation comparison (OS)

3.2.1. For the determination of oxides of lanthanum impurities of vanadium, iron, cobalt, manganese, copper, Nickel, titanium and chromium each sample comparison (OSOL) is prepared as follows: 30 g basics — oxide of lanthanum, clean at the designated impurities was placed in a quartz Cup, moisten with water, add 80 cmof nitric acid, diluted 1:1, dissolved by heating on the tile, enter the calculated number of appropriate solutions (see table.1), is evaporated to wet salts, treated twice with distilled water, evaporated to dryness, heated to remove the oxides of nitrogen and calcined in a muffle furnace at 900−950 °C for 2 h.

Each OS is then ground in a mortar made of organic glass for 1 h, periodically adding alcohol, maintaining the mixture in a pasty condition. Dry under an infrared lamp and calcined in a muffle furnace at 900−950 °C for 30−40 min. the Content of each of the designated impurities in ОСОЛ1-ОСОЛ5 and the amount of solution administered to a basis, are shown in table.1.

Table 1

(Changed edition, Rev. N 1).

3.2.2. For the determination of dioxide of cerium impurities of iron, cobalt, manganese, copper, Nickel, and chromium each sample comparison (OSI) is prepared as follows: 30 g fundamentals of cerium dioxide, pure at the designated impurities was placed in a beaker with a capacity of 600 cm, moisten with water, add 200 cmof nitric acid (1:1), dissolve by heating on the tile, gradually adding 120 cmof perhydrol, transferred into a platinum Cup and enter the calculated amount of the respective solutions (see table.2).

Then do as stated in claim 3.2.1.

Table 2

3.2.3. For the determination of dioxide of cerium impurities of vanadium and titanium each sample comparison (OOSC) is prepared as follows: 20 g fundamentals of cerium dioxide, pure vanadium and titanium, were placed in a glass with a capacity of 600 cm. Then do as stated in claim 3.2.2 using 150 cmof nitric acid, diluted 1:1, 80 cmof perhydrol, and the solutions are given in table.3.

Table 3

3.2.4. To determine the oxides of europium impurities of iron, cobalt, manganese, copper, Nickel, and chromium each sample comparison (OSOE) is prepared as follows: 20 g of europium oxide was placed in a platinum Cup, moisten with water, add 60 cmof nitric acid, diluted 1:1, dissolved by heating on the tile, enter the calculated amount of the respective solutions (see table.4), then do as stated in claim 3.2.1. The content of each of the designated impurities in ОСОЕ1-ОСОЕ5 and the amount of solution administered to a basis, are shown in table.4.

Table 4

3.2.4.1. To determine the oxides of europium impurities silicon, iron, copper and zinc each sample comparison (OSOE) is prepared as follows: 20 g of europium oxide was placed in a platinum Cup, then do as stated in claim 3.2.4. The content of each of these impurities in ОСОЕ6-ОСОЕ10 and the amount of solution administered to a basis, are shown in table.4A.

Table 4A

(Added, Rev. N 2).

3.2.5. Grinding in a mortar, and drying under a heat lamp are in the box of organic glass. Ready references stored in tightly closed cans of organic glass.

The mass fraction of each of the designated impurities shown in table.1−4, this in the calculation of the mass fraction of the respective metal in the mixture of metals and an appropriate framework — oxide REE.

3.2.6. Allowed preparation of samples comparison by mixing the oxides defined elements with an appropriate base (oxide REE) or according to GOST 23862.4−79 PP.3.1, 3.2, while maintaining the values of the mass fractions of the determined elements are listed in the table.1−4.

(Added, Rev. N 1).

3.2.7. For the determination of calcium in the oxides of gadolinium and yttrium, each comparison sample is prepared as follows: 10 g of the bases is placed in a quartz Cup, moisten with water, add 60−70 cmof nitric acid, diluted 1:1, dissolved by heating on the tile, enter the calculated amount of the respective solutions (table.4B), then do as stated in claim 3.2.1.

Table 4B

3.2.8. For determination of lutetium oxide contaminants cobalt, manganese, copper, Nickel, titanium and chromium each sample comparison (Solu) is prepared as follows: 20 g of lutetium oxide were placed in a quartz Cup, moisten with water, dissolved in 80−90 cmof nitric acid, diluted 1:1, enter the calculated quantity of appropriate solutions, then act as described in section 3.2.1. Mass fraction of each of the designated impurities in ОСОЛю1-ОСОЛю4 and the amount of solution administered to a basis, are shown in table.4B.

Table 4B

3.2.9. For the determination of oxides of yttrium impurities of magnesium and lead, each sample comparison (SDIO) is prepared as follows: 20 g of yttrium oxide were placed in a quartz Cup, moisten with water, add 70−90 cmof nitric acid, diluted 1:1, dissolved by heating on the tile, enter the calculated amount of the corresponding solution, then act as described in section 3.2.1. The content of magnesium and lead in ОСОИ1-ОСОИ4 and the amount of solution injected into the substrate, are shown in table.4G.

Table 4G

3.2.10. For the determination of oxides of yttrium impurity of cobalt in each sample comparison (Isoico) is prepared as follows: 20 g of yttrium oxide were placed in a quartz Cup, moisten with water, add 70−90 cmof nitric acid, diluted 1:1, dissolved by heating on the tile, enter the calculated amount of the corresponding solution of cobalt, then do as stated in claim 3.2.1. The content of cobalt in ОСОИКо1-ОСОИКо5 and the amount of solution administered to the basis given in table.4D.

Table 4D

3.2.11. For the determination of oxides of yttrium impurities of zirconium samples comparison prepared by mixing oxides of yttrium with zirconium dioxide. The head sample comparison (GOSIC) containing 10% zirconium, is prepared by mixing 135 mg of Zirconia with 865 mg of yttrium oxide in a mortar made of organic glass. The mixture was thoroughly triturated for 1 h, adding alcohol to maintain a pasty condition of the mass is dried in a drying closet at 100−110 °C for 1 h, and then calcined in a muffle furnace at 850−900 °C for 1 h. the Remaining samples of the comparison, prepare a serial dilution of GOSIC, and then each subsequent sample is the oxide of yttrium. Mass fraction of zirconium in the sample comparison and sample of an oxide of yttrium and the previous sample are given in table.4E.

Table 4E

3.2.7−3.2.11. (Added, Rev. N 2).

4. ANALYSIS

Metals transferred to the oxide according to GOST 23862.0−79.

4.1. Filling electrodes in the analysis of oxide of lanthanum

A portion of the sample (reference sample or base) with a mass of 300 mg was mixed with 150 mg of graphite powder in a mortar made of organic glass to obtain a homogeneous mixture. The resulting mixture was poured onto a sheet of tracing paper and repeated immersion in it electrodes I filled tightly to the brim of the craters of the five electrodes. In the same way craters five electrodes IV fill buffer mixture (p.3.1.1).

4.2. Filling electrodes in the analysis of cerium dioxide

4.2.1. In determining the impurities of iron, cobalt, manganese, copper and Nickel in the crater five electrodes II sequentially placed 2 mg of silver chloride and 50 mg of a sample (reference sample or base). Electrodes V fill buffer mixture (p.3.1.2) method set out in claim 4.1.

4.2.2. In the determination of impurities of vanadium and titanium 750 mg of a sample (reference sample or base) is mixed with 150 mg of powdered graphite. Craters five electrodes II is filled with the mixture (n.4.1).

4.3. Filling electrodes in the analysis of europium oxide

4.3.1. In determining the impurities of iron, cobalt, manganese, copper, Nickel, and chromium a portion of the sample (sample comparison, basics) with a mass of 200 mg was mixed with 200 mg of powdered graphite.

4.3.2. In the determination of impurities silicon, iron, copper and zinc weighed test portion (reference or basis) weight of 200 mg was mixed with 200 mg of buffer mix (p.3.1.3).

4.3.3. With this mixture fill the craters three electrodes III and craters three electrodes VII (p.4.1).

(Changed edition, Rev. N 2).

4.3. Filling electrodes in the determination of calcium in the oxides of gadolinium and yttrium

A portion of the sample (reference sample or base) weighing 150 mg was mixed with 150 mg of powdered graphite. Craters of the six electrodes VIII fill with the mixture (n.4.1).

4.3 b. Filling electrodes in the analysis of lutetium oxide

A portion of the sample (reference sample or base) of 50 mg mixed with 50 mg of powdered graphite. With this mixture fill the craters three electrodes IX (n.4.1).

4.3 V. the Filling of the electrodes in the analysis of oxides of yttrium

4.3 B. 1. In the determination of impurities of magnesium and lead a portion of the sample (reference sample or base) with a weight of 100 mg was mixed with 100 mg graphite powder. With this mixture fill the craters three electrodes VIII. A buffer mixture (p.3.1.2) fill the craters of the same three electrodes VIII (p.4.1).

4.3 B. 2. When determining the impurity of cobalt in the craters of the five electrodes sequentially placed IV 8 mg sodium chloride and 30 mg of the sample (reference sample or base) and carefully compacted with a kick ball made of organic glass. Craters five electrodes VIII fill (p.4.1) a buffer mixture (p.3.1.1).

4.3 B. 3. In determining the impurities of zirconium, a portion of the sample (reference sample or basis) weight of 160 mg was mixed with 80 mg of powder graphite. Craters three electrodes V is filled with the mixture (n.4.1).

4.3 a-4.3 V. 3. (Added, Rev. N 2).

4.4. Excitation and photography of the spectra

The excitation spectra are arc discharge between carbon electrodes. The spectra photographed with a spectrograph DFS-13 diffraction grating working in first order of reflection, with being with a lighting system. The conditions of excitation and photography of the spectra are shown in table.5. Used photographic plates of type II. Exposed photographic plates show washed in running water, fixed, washed in running water for 15 min and dried.

Table 5

(Changed edition, Rev. N 2).

5. PROCESSING OF THE RESULTS

5.1. In each spectrogram photometric blackening of analytical lines of the determined elements (table.6) and nearby background and calculate the difference of pochernenija . For all parallel values obtained on the spectrograms taken for each sample, find the average value .

Table 6

(Changed edition, Rev. N 1, 2).

5.2. If the analytical line of the designated element in the spectra of samples basis of comparison is missing, then, using the values and for samples comparison, build a calibration curve in the coordinates (, ). In these graphs by values of the samples determine the content of impurities in the sample.

Discrepancies in the results of the two tests should not exceed the values of permissible differences given in table.7.

5.3. If in the spectra of samples basis of comparison, there is a weak line of the element, then the construction of calibration curve, corrected for the value of the mass fraction of the element in the sample comparisons. An amendment is permissible only under the condition that this value does not exceed the specified for the method lower limit of determination.

(Changed edition, Rev. N 1).

5.4. Under the control of the reproducibility of parallel measurements of all values of the analytical parameters obtained for all the spectrograms of a sample, select the largest and smallest value and find the schedule for the calibration values , and  — the largest and the smallest results of parallel measurements of impurities in the sample. The differences between them (the ratio of more to less) should not exceed values of allowable differences specified in table.7.

Table 7

(Changed edition, Rev. N 2).

5.5. When you control the accuracy of using GSO 2820−83 proceed as follows.

5.5.1. In the analysis of the lanthanum oxide sample of GSO with a mass of 150 mg was mixed with 300 mg base, then carry out the analysis, as specified in PP.4.1, 4.4, 5.1−5.4. The result of the analysis () is considered correct if the ratio values and (calculate the ratio of largest to smallest) satisfies the condition p. 18 GOST 23862.0−79.

5.5.2. In determining the vanadium and titanium to cerium oxide suspension GSO with a mass of 150 mg, is mixed with 750 mg base, then carry out analysis as specified in PP.4.2.2, 4.4, 5.1−5.4. The result of the analysis () is considered correct if the ratio values and (calculate the ratio of largest to smallest) satisfies the condition p. 18 GOST 23862.0−79.

5.5.3. In the determination of iron, cobalt, manganese, copper, Nickel, and chromium in oxide europium sample of GSO with a mass of 200 mg was mixed with 200 mg base. In the determination of silicon, iron, copper and zinc oxide europium sample of GSO with a mass of 198 mg mixed with 2 mg of sulfur, and 200 mg base. Next, carry out analysis as specified in PP.4.3.3, 4.7, 5.1−5.4.

The result of the analysis () is considered correct if the ratio values and (calculate the ratio of largest to smallest) satisfies the condition p. 18 GOST 23862.0−79.

5.5.4. In the determination of calcium in the oxides of gadolinium and yttrium a portion of the bonds a weight of 150 mg was mixed with 150 mg base. Next, carry out analysis as specified in PP.4.4, 4.7, 5.1−5.4. The result of the analysis () is considered correct if the ratio values and (calculate the ratio of largest to smallest) satisfies the condition p. 18 GOST 23862.0−79.

5.5.5. In the analysis of lutetium oxide weighed GSO with a mass of 50 mg mixed with 50 mg base. Next, carry out analysis as specified in the PP.4.3 b, 4.4, 5.1−5.4. The result of the analysis () is considered correct if the ratio values and (calculate the ratio of largest to smallest) satisfies the condition p. 18 GOST 23862.0−79.

5.5.6. In the analysis of oxides of yttrium: in the determination of magnesium and lead a portion of the bonds with a weight of 100 mg was mixed with 100 mg base. Next, carry out analysis as specified in the PP.4.3 B. 1, 4.4, 5.1−5.4. The result of the analysis () is considered correct if the ratio values and (calculate the ratio of largest to smallest) satisfies the condition p. 18 GOST 23862.0−79.

In determining the zirconium weighed GSO with a mass of 80 mg was mixed with 160 mg base. Next, carry out analysis as specified in the PP.4.3 B. 3, 4.4, 5.1−5.4. The result of the analysis () is considered correct if the ratio values and (calculate the ratio of largest to smallest) satisfies the condition p. 18 GOST 23862.0−79.

5.5−5.5.6. (Added, Rev. N 2).