Reagents. Copper II Sulphate Pentahydrate. Specification.

Reagents. Copper II Sulphate Pentahydrate. Specification.
This standard shall apply to copper II sulphite pentahydrate, which represents itself as a
blue crystal powder, soluble in water, diluted alcohol, concentrated hydrochloric acid and is exposed to air
efflorescence.
Document description:
GOST 4165-78
INTERSTATE STANDARD
REAGENTS
Copper II Sulphate Pentahydrate.
SPECIFICATION
Official edition
Standard Publishers Publishing and Printing Complex.
Moscow
UDC 546.56’226-41:006.354
Group L51
INTERSTATE STANDARD
REAGENTS
GOST
Copper II Sulphate Pentahydrate
4165-78
Specification
Russian National Product Classifier (RNPC): 26 2224 0330 03
Date of implementation: 01/01/79
This standard shall apply to copper II sulphite pentahydrate, which represents itself as a blue crystal
powder, soluble in water, diluted in alcohol, concentrated hydrochloric acid and is exposed to air
efflorescence.
Formula: CuSO4 5H2O.
Relative molecular mass (in accordance with International Atomic Mass Classifier as of year 1987) –
249.69.
It is acceptable to fabricate copper II sulphate pentahydrate in compliance with ISO 6353-2-83 (P.9)
(Adendum 1) and carry out analysis under ISO 6353-1-82 (Addendum 2).
(Edited revision, edits # 2, 3).
1. SPECIFICATION
1.1
Copper sulphite pentahydrate shall be fabricated in accordance with requirements of the
current standard under process reglament approved in an established manner.
1.2
Copper II sulphite pentahydrate physical and chemical profile is to comply with the norms
and requirements indicated in the Table below.
Normal value
Index Description
Chemically clean (ch.c.)
RNPC 26 2224 0333 00
Clean for analysis purposes
(c. a. p.)
Clean (c.)
RNPC 26 2224 0331 02
RNPC 26 2224 0332 01
1.Mass fraction of copper II
sulphite pentahydrate
(CuSO4 5H2O), % , up to
99.5
99.5
98.5
2.Mass fraction of water
insoluble impurities, %, up
to
0.002
0.004
0.008
3.Mass fraction of total
nitrogen (N), %, up to
0.001
0.002
0.008
4.Mass fraction of chlorides
(Cl), %, up to
0.0005
0,0005
0.0050
5.Mass fraction of iron (Fe),
%, up to
0.001
0,005
0.020
6.Mass fraction of arsenic
(As), %, up to
0.0005
0.0005
Not rated
7.Mass fraction nonsulphate settleable solids by
H2S contact, up to
0.05
0.10
0.20
8.Mass fraction of nickel
(Ni), %, up to
0.002
Not rated
(Edited revision, edits # 1, 2, 3).
Official edition
Reprinting prohibited
© Standard Publishers, 1978
© Standard Publishers Publishing and Printing Complex, 2001
P. 2 GOST 4165-78
2. RULES OF ACCEPTANCE
2.1
Rules of acceptance – under GOST 3885.
2.2
Manufacturer shall perform mass fraction identifications of chlorides, total nitrogen and non-sulphate
settleable solids by H2S contact in each 20-th product batch.
(Additionally introduced, edit #2).
3. ANALYSIS METHODS
3.1a.
Common guidelines to analysis performance – under GOST 27025.
General purpose laboratory scales, types VLR-200g, VLKT – 500g or VLE-200g shall be used for weighing.
It is acceptable to use other means of measuring fitted with metrological characteristics and equipment
with technical characteristics as good as those proposed, as well as reagents with quality features no lower
than those stipulated in this standard.
(Edited revision, edits # 2, 3).
3.1
Sampling is to comply with GOST 3885. Average sample mass weight shall be as minimum as 300g.
(Edited revision, edits # 2, 3).
3.2
Mass fraction identification of copper II sulphate pentahydrate
3.2.1 Hardware, reagents and solutions
Drop tube with a capacity of 50cm3 and scale division of 0.1cm3.
Test flask, ‘Ki-2-250-43, TKhS’ type to GOST 25336.
Scaled droppers with a capacity of 2.5 and 10cm3.
Glass ‘SV-14/8’ to GOST 25336.
Cylinder 1(3)-100-2 to GOST 1770.
Distilled water to GOST 6709.
Potassium iodide to GOST 4232, chem. clean.
Acetic acid to GOST 61, glacial, chem.. clean.
Soluble starch to GOST 10163, solution with a mass fraction of 1%.
Sodium thiosulphate pentahydrate to GOST 27068, solution with a molarity of (Na2S2O3 5H2O) =0.1
mol/dm3 (0.1 n); preparation to GOST 25794.2.
(Edited revision, edits # 2, 3).
3.2.2 Analysis procedure
Place 1.0000g of preparation inside a test flask and dissolve in 50cm3 of water. Then add 5cm3 of
acetic acid, 3g of potassium iodide, mix it and titrate against sodium thiosulphate pentahydrate from drop
tube, adding 2cm3 of starch solution at the end of titration.
(Edited revision, edit # 2).
3.2.3 Processing results
Mass fraction of copper II sulphate pentahydrate (X) is calculated through the following formula:
Where V is a volume of sodium thiosulphate pentahydrate solution used for titration with molarity
exactly equal to 0.1 mol/dm3;
m is a mass of sample weight in g;
0.02497 is a mass weight of copper II sulphate pentahydrate, corresponding to 1cm3 of sodium thiosulphate
solution with with molarity exactly equal to 1 mol/dm3.
The analysis result is corrected to mass weight of iodates in used volume of potassium iodide, which is
defined through blank test.
The analysis result is elicited out of arithmetic average result of three parallel identifications, where
absolute discrepancy of the most different values shall not exceed the allowable deviation margin, which is
0.3%.
Allowable absolute cumulative accuracy of the analysis result is ±0.4% at confidential probability
P=0.95.
(Edited revision, edits # 2, 3).
GOST 4165-78 P. 3
Mass fraction identification of water insoluble impurities
3.3.1 Hardware, reagents and solutions
Glass, ‘V-1-600 TKhS’ to GOST 25336.
Filter crucible, type TF POR 10 or TF POR 16 to GOST 25336.
Cylinder ‘1-500-2’ or dram glass vial 500 to GOST 1770.
Distilled water to GOST 6709.
Sulfuric acid to GOST 4204, 20% mass fraction solution.
3.3.2 Analysis procedure
Place 50.00g of preparation in a glass and dilute with 300cm3 of water, preheated to 60°C and acidified
with 1cm3 of sulfuric acid. Filter the solution through the crucible that had been preliminarily dried to its stable
mass and weighed (record the outcome in grams with accuracy to the fourth decimal digit). Rinse the residue
substance with 150gr of hot water and dry out in a drying cabinet at 105-110°C until reaching a stable mass.
The preparation is considered compliant to present standard requirements if the residue mass after dry out
does not exceed the following:
for preparation, chemically clean – 1 mg,
for preparation, clean for analysis purposes – 2mg,
for preparation, clean – 4mg.
Allowable absolute cumulative accuracy of the analysis result is ±30% for ch. c. & c. a. p. qualified
preparations and ± 15% for c. qualified preparation at confidential probability P=0.95.
3.3.1, 3.3.2 (Edited revision, edits # 2, 3).
3.4
Mass fraction identification of total nitrogen
The identification is to be carried out under GOST 10671.4. For this purpose, place 2.00g of preparation,
chemically clean or 1.00 of preparation, clean for analysis purposes / clean in a dram glass vial K-2-250-34
‘TKhS; (GOST 25336), dissolve in 50 cm3 and then follow visual color-metric method for identification.
The preparation is considered compliant to present standard requirements if the color of sample solution is
not more intensive than the color of the solution prepared simultaneously with the one analyzed and that
contains the same following volumes:
for preparation, chemically clean – 0.02 mg N,
for preparation, clean for analysis purposes – 0.02mg N,
for preparation, clean – 0.08mg, N.
1cm3of sodium hydroxide and 1 cm3 of Nessler’s or Nessler and Winkler’s reagent.
(Edited revision, edit # 2).
3.5
Mass fraction identification of total chlorides
The identification is to be carried out under GOST 10671.7. For this purpose, place 5.00 grams of
preparation in a 100 cm3 capacity measuring flask, dissolve in 50 cm3 of water, add 10 cm3 of sulfuric acid
solution with a mass fraction of 25%, make up the volume to the mark-up point and mix. Then filter the
3.3
solution through ashless “blue ribbon” type filter that had been preliminarily flushed by nitric acid solution
with a mass fraction of 1%.
Place 20 cm3 of solution obtained (corresponding to 1g of preparation) in a 100 cm3 capacity cone
flask, make up the solution volume to 39 cm3 and then follow visual color-metric method for identification in
the volume of 40 cm3 without adding nitric acid.
The preparation is considered compliant to present standard requirements if opalescence of sample
solution is not more intensive than the opalescence of the solution prepared simultaneously with the one
analyzed and that contains the same following volumes: 20 cm3 of copper (II) sulphate pentahydrate solution
not containing chlorides:
for preparation, chemically clean – 0.005mg Cl,
for preparation, clean for analysis purposes – 0.005mg Cl,
for preparation, clean – 0.050mg, Cl.
And 1 cm3 of silver nitrate.
Copper (II) sulphate pentahydrate solution not containing chlorides is prepared the following way:
place 5.00 grams of preparation in 100 cm3 capacity measuring flask, dissolve in 50 cm3 of water, add 10 cm3 of
nitric acid with a mass fraction of 25%, 5 cm3 of silver nitrate solution, make up the volume to the mark-up
point, mix and leave in a dark place for 12 hours.
Then filter the solution through ashless “blue ribbon” type filter that had been preliminarily flushed by
nitric acid solution with a mass fraction of 1%.
(Edited revision, edits # 1, 2).
P. 4 GOST 4156-78
3.6
Mass fraction identification of iron
The identification is to be carried out under GOST 10555. For this purpose, place 2.00 grams of
preparation in a 100 cm3 capacity glass and then follow sulphosalicylic method having preliminarily segregated
iron by ammonia solution in presence of ammonium chloride and diluting sediment on 3 cm3 hydrochloric acid
filter, instead of 2 cm3. Collect filtrate and rinsewaters in a 100 cm3 capacity measuring flask, use water to make
up the solution to the mark-up point and mix.
For analysis purposes, take 25 cm3 of solution obtained (corresponds to 0.5g of preparation) for
preparation, chemically clean and clean for analysis purposes or 12.5 cm3 (corresponds to 0.25g of preparation)
for preparation, clean. Carry out identification without adding hydrochloric acid.
The preparation is considered compliant to present standard requirements if the iron mass weight does
not exceed the following:
for preparation, chemically clean – 0.005mg,
for preparation, clean for analysis purposes – 0.025mg,
for preparation, clean – 0.050mg.
The analysis result is corrected to mass weight of iron in used volumes of reagents, which is defined
through blank test.
It is acceptable to finalize identification visually.
Should there be any discrepancies in iron mass weight identification the analysis is finalized via
photometric measurement.
3.7
Mass fraction identification of arsenic
The identification is to be carried out under GOST 10485. For this purpose, place 0.50g of preparation
in a 100 cm3 capacity cone flask, dissolve in 40 cm3 of water, add 1 cm3 of concentrated nitric acid (GOST
4461), heat up and leave boiling for 1-2 minutes. In the hot solution add 2 cm3of ferrous ammonium sulfate
solution with mass fraction of 1%, then while mixing add ammonia solution with mass fraction of 25% until
the sediment of copper subsalt is fully dissolved. Then add 2 cm3 of excess ammonia solution, bring the
solution to the boil and leave on boiling water bath for 30 minutes.
Filter the solution through ashless “white ribbon” type filter. Rinse the sediment with 100 cm3 of hot
water containing 2 cm3 ammonia solution until the full disappearance of blue color sediments on the filter,
disposing of filtrate and rinsewaters.
Dilute the filter sediment with 20 cm3 of hot sulfuric acid.
Place 4 cm3 of solution obtained (corresponding to 0.10g of preparation) in a test flask of arsenic
identification apparatus. Then identification is carried out by means of a visual method using mercuric bromide
paper in sulfuric acid media, adding 16 cm3 of sulfuric acid instead of 20 cm3.
The preparation is considered compliant to present standard requirements if the color of mercuric
bromide paper out of sample solution is not more intensive than the color of mercuric bromide paper out of the
solution prepared simultaneously with the one analyzed and containing 0.0005mg As, 20 cm3 sulfuric acid
solution, 0,5 cm3 tin dichloride dihydrate and 5g of zynk in the same volume.
3.6, 3.7 (Edited revision, edits # 2, 3).
3.8
Mass fraction identification of non-sulphate settleable solids by H2S contact
3.8.1 Hardware, reagents and solutions
Test flask ‘Ki-2-250-43, TKhS’ type to GOST 25336.
Scaled dropper with a capacity of 10cm3.
Cylinders, 1(3)-250-2 and 1(3)-100-2 to GOST 1770
Bowl 100 to GOST 19908.
Evaporation bowl 3 to GOST 9147.
Distilled water to GOST 6709.
Sulfuric acid to GOST 4204, solution with mass fraction of 20%; preparation under GOST 4517.
Hydrogen sulphide
3.8.2 Analysis performance
Place 10.00g of preparation in a test flask (with a mark-up at 150 cm3) and dilute in 140 cm3 of water. Add
10 cm3 of sulfuric acid and heat up the solution to 70-80°C. Place the test flask in the hot water bath and slowly
introduce hydrogen sulphide until sulfuric copper is fully settled (test to establish settlement completion). Then
make up the solution volume to the mark-up and mix. Once the solution is cool and settled, promptly filter it
through the folded filter by completely filling it with the filtered liquid (to prevent possible sulfuric copper
oxidizing resulting in copper and filtrate entrainment).
GOST 4165-78, P.5
Use cylinder 1(3)-`00-2 to place 75 cm3 of filtrate (corresponding to 5g of preparation) in evaporation bowl
or quartz bowl once the latter is conditioned the latter to constant mass weight and weighed (record the
outcome in grams with an accuracy to the fourth decimal digit). Do the steam-out on water bath first, then on
sand bath until sulfuric acid fumes do not extract any longer. Bake the residue in the muffle furnace at 500 600°C until a constant mass weight is achieved.
The preparation is considered compliant to present standard requirements if the residue mass weight after
baking does not exceed the following:
for preparation, chemically clean – 2.5mg,
for preparation, clean for analysis purposes – 5.0mg,
for preparation, clean – 10.0mg
Keep the residue to identify mass fraction of nickel per par. 3.9.
Allowable relative cumulative accuracy of the analysis result is ±15% at confidential probability P=0.95
3.8.1, 3.8.2 (Edited revision, edits # 2, 3).
3.9
Mass fraction identification of nickel
3.9.1
Hardware, reagents and solutions
Scaled dropper with a capacity of 2.5 or 10cm3.
Vial ‘P1-16-150 KhS’ to GOST 25336.
Cylinders 1(3)-25-2 to GOST 1770.
Aqueous ammonia to GOST 3760, solution with mass fraction of 10%.
Di-ammonium hydrogen citrate, solution with mass fraction of 10%.
Bromine to GOST 4109, saturated aqueous solution (bromine water); preparation under GOST 4517.
Distilled water to GOST 6709.
Dimethyi glioxime to GOST 5828, alcohol solution with mass fraction of 1%; preparation under
GOST 4517.
Nitric acid to GOST 4461.
Hydrochloric acid to GOST 3118, concentrated and solution with mass fraction of 25%; preparation
under GOST 4517.
Ni containing solution; preparation under GOST 4212; solution with mass concentration of 0.01mg/
cm3 Ni is achieved through corresponding dilution.
Rectified ethyl alcohol, technical premium grade to GOST 18300.
Mixture of acids: preparation through mixing concentrated nitric and hydrochloric acids in 1:3 ratio
by volume.
(Edited revision, edits # 2, 3).
3.9.2 Analysis performance
Add 4 cm3 of acid mixture to the residue obtained per par. 3.8 and steam out dry on a water bath.
Dilute the residue in 1 cm3 of hydrochloric acid solution with mass fraction of 25% and 19 cm3 of water,
then filter it through ashless “blue ribbon” type filter.
Place 2 cm3 of solution obtained (corresponding to 0,5g of preparation) in a vial of plain glass, then
while mixing add 2 cm3 of di-ammonium hydrogen citrate, 1 cm3 of bromine water, 7 cm3 of aqueous
ammonia and 3 cm3 of dimethyi glioxime.
(Edited revision, edit # 2).
P. 6 GOST 4165-78
4. PACKAGING, IDENTIFICATION, TRANSPORTATION AND STORAGE
4.1
Packaging and identification of the preparation shall comply with GOST 3885.
Package view and type: 2-1, 2-2, 2-4, 2-9, 6-1, II-1, II-6.
Prepackaging group: IV, V, VI, VII.
Cargo classification reference to GOST 19433-9153.
(Edited revision, edits # 1, 2, 3).
4.2
Preparation delivery is arranged by all means of transport in accordance with the Rules for Cargo
Transportation applicable to specific type of transport.
4.3
Preparation shall be stored in original Manufacturer’s package in covered warehouse
accommodations.
5. MANUFACTURER’S WARRANTY
5.1
Manufacturer guarantees compliance of the preparation to the present standard requirements provided
that transportation and storage conditions are observed.
5.2
Preparation storage warranty period is two years as of the date of fabrication.
5.1, 5.2 (Edited revision, edit # 1).
6.
SAFETY REQUIREMENTS
6.1
Copper (II) sulphate pentahydrate is a non-flammable toxic substance. In case of digestion it causes
poisoning, in contact with skin and muscous membranes is causes irritation. The level of exposure on a human
organism is equal to substance severity Class 2 (GOST 12.1.007). Maximum permissible concentration of the
substance in workplace air is 0.5mg / cm3 (based on copper).
6.2
While working with the preparation, personal protection equipment shall be used in accordance with
industrial type norm. Also, personal hygiene rules shall be observed.
6.1, 6.2 (Edited revision, edits # 2, 3).
6.3
All premises where the preparation is used are to be equipped with continuously operated draft
ventilation. The preparation laboratory analysis is to be carried out inside an extract hood.
(Edited revision, edit # 3).
GOST 4165-78 C. 7
ADDENDUM 1
Compulsory
ISO 6353-84 Reagents for chemical analysis. Part 2. Specification. First series.
P.9 Copper (II) sulphate pentahydrate. Relative molecular weight is 249.68.
P.9.1 S p e c i f i c a t i o n
Copper sulphate pentahydrate mass fraction.
(II) (CuSO4 5H2O) %, as min as
99.0
Mass fraction of chlorides (Cl), %, up to
0.00
1
Mass fraction of total nitrogen (N), %, up to
0.00
3
Mass fraction of iron (Fe), %, up to
0.00
5
Mass fraction of nickel (Ni), %, up to
0.00
5
Mass fraction of potassium, (K), %, up to
0.00
1
Mass fraction of sodium (Na), %, up to
0.00
5
Mass fraction of zinc (Zn), %, up to
0.05
P 9.2 P r e p a r a t i o n o f s a m p l e s o l u t i o n
Dissolve 10g of preparation in 50 cm3 of water and dilute to 100 cm3.
P. 9.3 A n a l y s i s m e t h o d s
P9.3.1 Mass fraction identification of copper (II) sulphate pentahydrate.
Weigh in about 1.000 of preparation and dissolve in 60 cm3 of water.
Add 5 cm3 of sulfuric acid solution with mass fraction of 20% and 3g of potassium iodide.
Titrate educed iodine with sodium thiosulphate with molarity exactly equal to (Na2S2O3) = 0.1 mol/dm3, then
add starch solution at the end of titration.
Starch solution shall be prepared as follows: using 1.0g of soluble starch and 5 cm3 of water prepare a
paste. Boil in 100 cm3 of hot boiling water for 1-2 minutes while mixing the solution then leave for cooling.
The solution may be used within two weeks. (The solution due date may be extended up to several months by
adding several drops of formaldehyde.)
1.00 cm3 of sodium thiosulphate with molarity exactly equal to (Na2S2O3) = 0.1 mol/dm3 corresponds
to 0.02497g of CuSO4 5H2O.
P. 9.3.2 Mass fraction identification of chlorides
Make up 10 cm3 of sample solution (P9.2) to 20 cm3 with water and analyze in compliance with
GM2*.
Prepare reference solution by using 1 cm3 of reference chloride containing solution II)1 cm3 = 0.001%
Cl).
Prepare reference chloride containing solution II in a measuring flask straight before it is used by
diluting base reference solution with water in 1:100 ratio. Base reference solution shall be prepared the
following way: dissolve 1.65g of NaCl in water, make up with water to mark-up point on a 1000 cm3 capacity
measuring flask and mix.
P.9.3.3. Mass fraction identification of total nitrogen
Analyze 10 cm3 of sample solution (P.9.2) in compliance with GM 6*.
Prepare reference solution by using 3 cm3 of reference nitrogen containing solution II (3 cm3
=0.003%N).
Prepare reference nitrogen containing solution II in a measuring flask straight before it is used by
diluting base reference solution with water in 1:100 ratio. Base reference solution shall be prepared the
following way: dissolve 6.07g of NaNO3 in water, make up with water to mark-up point on a 1000 cm3 capacity
measuring flask and mix.
P.9.3.4. Mass fraction identification of iron
Add 5 cm3 of hydrochloric acid and 1 drop of nitric acid to sample solution (P9.2). Extract 2- cm3 of 4methyl-2- penthanon and flush organic phase of 10 cm3 hydrochloric acid with mass fraction of 25%.
Extract iron from the organic phase of 20 cm3 of water. Segregate water phase and analyze in compliance with
GM 8.1*.
Prepare reference solution by using 5 cm3 of reference iron containing solution II (5 cm3=0.005% Fe).
Prepare reference iron containing solution II in a measuring flask straight before it is used by diluting
base reference solution with water in 1:100 ratio. Base reference solution shall be prepared the following way:
add 10 cm3 of sulfuric acid with mass fraction of 25% to 8.63g of NH4Fe(SO4)2 12H2O, make up with water to
mark-up point on a 1000 cm3 capacity measuring flask and mix.
P.9.3.5. Mass fraction identification of nickel and zinc
Identification is achieved through atomic-absorption spectroscopy method in compliance with GM 29*
at the following conditions:
*General Methods of Analysis (GM) – to ISO 6353-1-82.
P. 8 GOST 4165-78
Element
Solution concentration, %
N1
Zn
Element
1%
Flame
Air-acetylene
Resonance line, nm
232.0 or 325.5
589.0
Mass fraction identification of potassium and sodium
Identification is achieved through flame photometry method in compliance with GM 30* at the
following conditions:
Solution concentration, %
Flame
Wave length, nm
K
766.5
Sample solution (P.9.2)
Oxygen-acetylene
Na
589.0
ADDENDUM 2
Compulsory
ISO 6353-1-82 Chemical reagents. Part 1. General test methods.
5.2
Mass fraction identification of chlorides (GM 2)
Use a defined volume of sample analysis acidified by 1 cm3 of nitric acid with mass fraction of 25%
and add 1 cm3 of silver nitrate with mass fraction of approximately 1.7%.
Leave the mixture to settle for 2 min, then compare its opalescence with the opalescence of mixture
obtained through similar treatment of a corresponding reference solution.
5.6
Mass fraction identification of total nitrogen (GM 6)
Use a defined volume of sample solution that had been diluted, if necessary to the volume of 140 cm3
in Kjeldahl apparatus comprised by Kjeldahl flask and distillation unit. Add 5 cm3 of sodium dioxide with mass
fraction of 32% and 1.0g of Devardo’s alloy or aluminum wire. Leave to settle for 1 h. Distill of 75 cm3 of
reaction mixture in a measuring cylinder containing 5 cm3 of sulfuric acid solution with mass fraction of 0.5%.
Add 3 cm3 of sodium dioxide with mass fraction of 32%, 2 cm3 of Nessler’s reagent and dilute to the volume of
100 cm3.
Compare the yellow color intensity of solution obtained with the one of the solution obtained through
similar treatment of a corresponding reference solution.
5.8.1. Mass fraction identification iron using 1.10-phenanthroline (GM 8.1) to GOST 10555.
5.29 Atomic-absorption spectroscopy (GM 29)
5.29.1 General guidelines
Sample preparation or its solution is taken into high-temperature flame created by suitable mixture of
flammable gas and flame supporting gas, thus providing evaporation of the sample preparation and
dissociation of its molecules to atoms. One may use a non-flame heating apparatus. The source representing
itself as a vacuum tube with a hollow cathode or electrodeless discharge tube activate by microwave radiation
produces radiation with a wave length corresponding to the atom excitation energy of analyzed substance. As
atoms of the element identified absorb a certain portion of the radiation proportionally equal to their number in
general (not excited) state, the absorption is registered by a suitable atomic absorption spectrometer.
5.29.2 Analysis methodology
Due to method essence, variety of existing devices, abundance of parameters related to analyzed sample and
the device as well as multiple of influential factors make it is impossible to provide detailed guidelines.
__________________________
*General Methods of Analysis (GM) – to ISO 6353-1-82.
GOST 4165-78 P.9
Methodology selection is defined by the degree of required accuracy. Possibility of distortions coming
from flame or non-flame type sources should be taken into account. If a device is supplied with flame atom
source, the identification is usually performed using aqueous solutions of analyzed substances that are slightly
acidified with nitric or hydrochloric acids.
With intent of registering the solution effects it is recommended to use spiking method. With the
method, the identification is done on aliquot series (its size depends on the degree of accuracy, though it must
be as minimum as two) of a solution under test with added known amounts of the substance identified.
Wave lengths corresponding to resonance lines as well as other specific data are provided in reagent
specific descriptions.
5.30. Flame photometry (GM 30)
5.30.1. General guidelines
This method is based on measuring the intensity of light radiation emitted by certain atoms in course of
their transition from excited state to the state with lower energy. Atoms turn to excited condition in flame
created by suitable mixture of flammable gas and flame supporting gas. The intensity of radiation emitted by
atoms is measured by a suitable photometric system equipped by a monochromator or filters.
N o t e : One may use other gas mixtures for flame than those listed here. In this case, the solution
concentrations recommended in the same descriptions might have to be corrected accordingly.
5.30.2. Analysis methodology.
Analysis methodology is similar to the one belonging to atomic absorption spectroscopy and here it is
also possible to provide general guidelines only. The conditions for each separate analysis are provided in
reagent specific descriptions.
ADDENDUMS 1, 2 (Introduced additionally, edit #3).
P. 10 GOST 4165-78
INFORMATION DATA
1. DEVELOPED AND INTRODUCED BY the Ministry of Chemical Industry of the USSR.
2. APPROVED AND IMPLEMENTED BY the Decree of the USSR Board of Ministers State
Standard Committee as of
3. SUPERSEDES GOST 4165-68
4. REFERENCE REGULATORY AND TECHNICAL DOCUMENTS
Description of referenced
Regulatory/Technical document
GOST 12.1.007-76
GOST 61-75
GOST 1770-74
GOST 3118-77
GOST 37360-79
GOST 3885-73
GOST 4109-79
GOST 4204-77
GOST 4212-76
GOST 4232-74
GOST 4461-77
GOST 4517-87
GOST 5828-77
GOST 6709-72
Par. subpar. .
#
6.1
3.2.1
3.2.1; 3.3.1;
3.8.1; 3.9.1
3.9.1
3.9.1
2.1; 3.1; 4.1
3.9.1
3.3.1; 3.8.1
3.9.1
3.2.1
3.7; 3.9.1
3.8.1; 3.9.1
3.9.1
3.2.1; 3.3.1;
3.8.1; 3.9.1
Description of referenced
Regulatory/Technical document
GOST 9147-80
GOST 10163-76
GOST 10485-75
Par. subpar. . #
GOST 10555-75
GOST 10671.4-74
GOST 10671.7-74
GOST 18300-87
GOST 19433-88
GOST19908-90
GOST25336-82
3.6; addendum 2
3.4
3.5
3.9.1
4.1
3.8.1
3.2.1; 3.3.1; 3.4;
3.8.1; 3.9.1
3.2.1
3.1a
3.2.1
GOST 25794.2-83
GOST 27025-86
GOST 27068-86
3.8.1
3.2.1
3.7
5. Validity limitation eliminated by the Decree of Gosstandart as of 24/09/92 # 1264
6. EDITION (October 2001) with Edits # 1, 2, 3 approved in February 1984, March 1988,
September 1992 (IUS 5-83, 6-88, 12-92).