GOST R 55558-2013

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  ГОСТ Р 55558-2013

GOST R 55558−2013 Ore copper-Nickel sulfide. Mass-spectrometric method for the determination of platinum, palladium, rhodium, ruthenium, iridium, and gold with pre-collectormania in Nickel matte

GOST R 55558−2013

NATIONAL STANDARD OF THE RUSSIAN FEDERATION

ORE COPPER-NICKEL SULFIDE

Mass-spectrometric method for the determination of platinum, palladium, rhodium, ruthenium, iridium, and gold with pre-collectormania in Nickel matte

Sulfide Copper-Nickel Ore. Mass-Spectrometry Method for Determination of Platinum, Palladium, Rhodium, Ruthenium, Iridium and Gold Content with Collecting Preliminary for Nickel Matte

OKS 77.120.40

Date of introduction 2014−07−01

Preface

1 was DEVELOPED by limited liability company «Institute Gipronikel '" (JSC «Gipronikel ' Institute»)

2 SUBMITTED by the Technical Committee for standardization TC 370 «Nickel. Cobalt"

3 APPROVED AND put INTO EFFECT by the Federal Agency for technical regulation and Metrology from August 28, 2013 N 836-art.

4 INTRODUCED FOR THE FIRST TIME


Application rules of this standard are established in GOST R 1.0−2012 (section 8). Information about the changes to this standard is published in the annual (as of January 1 of the current year) reference index «National standards» and the official text changes and amendments — in monthly information index «National standards». In case of revision (replacement) or cancellation of this standard a notification will be published in a future issue of information index «National standards». Relevant information, notification and lyrics are also posted in the information system of General use — on the official website of the Federal Agency for technical regulation and Metrology on the Internet (gost.ru)

1 Scope

This standard applies to ore copper-Nickel sulfide and sets the mass-spectrometric method of determining the content of platinum, palladium, rhodium, ruthenium, iridium and gold after collecting birds on Nickel matte.

2 Normative references

This standard uses the regulatory references to the following standards:

GOST 8.315−97 State system for ensuring the uniformity of measurements. Standard samples of composition and properties of substances and materials. The main provisions of the

GOST R 8.563−2009 State system for ensuring the uniformity of measurements. Techniques (methods) of measurements

GOST 12.0.001−82 standards System of labor safety. The main provisions of the

GOST 12.0.003−74 System safety standards. Dangerous and harmful production factors. Classification

GOST 12.0.004−90 System of standards of occupational safety. Organization of training safety. General provisions

GOST 12.1.004−91 System safety standards. Fire safety. General requirements

GOST 12.1.005−88 standards System of labor safety. General hygiene requirements for working zone air

GOST 12.1.007−76 System of standards of occupational safety. Harmful substances. Classification and General safety requirements

GOST 12.1.014−84 System of standards of occupational safety. The air of the working area. Method of measuring concentrations of harmful substances indicator tubes

GOST 12.1.016−79 System of standards of occupational safety. The air of the working area. Requirements for measurement techniques of concentrations of harmful substances

GOST R 12.1.019−2009 System of standards of occupational safety. Electrical safety. General requirements and nomenclature of types of protection

GOST 12.1.030−81 System of standards of occupational safety. Electrical safety. Protective grounding, neutral earthing

GOST 12.2.007.0−75 System safety standards. Products electrical. General safety requirements

GOST 12.3.002−75 System safety standards. The process of production. General safety requirements

GOST 12.3.019−80 standards System of labor safety. Test and measurement electrical. General safety requirements

12.4.009 GOST-83 System of standards of occupational safety. Fire fighting equipment for protection of objects. Principal. The accommodation and service

GOST 12.4.021−75 System safety standards. System ventilation. General requirements

GOST 1770−74 laboratory Glassware measuring glass. Cylinders, beakers, flasks, test tubes. General specifications

GOST 4204−77 Reagents. Sulphuric acid. Specifications

GOST 4212−76 Reagents. Methods of preparation of solutions for colorimetric and nephelometric analysis

GOST 4331−78 Reagents. Nickel oxide black. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 5679−91 Wool, cotton, clothing and furniture. Specifications

GOST R ISO 5725−1-2002 Accuracy (trueness and precision) of methods and measurement results. Part 1. The main provisions of the

GOST R ISO 5725−2-2002 Accuracy (trueness and precision) of methods and measurement results. Part 2. The basic method for the determination of repeatability and reproducibility of a standard measurement method

GOST R ISO 5725−3-2002 Accuracy (trueness and precision) of methods and measurement results. Part 3. Intermediate indicators the precision of a standard measurement method

GOST R ISO 5725−4-2002 Accuracy (trueness and precision) of methods and measurement results. Part 4. The main methods of determining the correctness of a standard measurement method

GOST R ISO 5725−5-2002 Accuracy (trueness and precision) of methods and measurement results. Part 5. Alternative methods for determining the precision of a standard measurement method

GOST R ISO 5725−6-2002 Accuracy (correctness and precision) of methods and measurement results. Part 6. The use of precision values in practice

GOST 5848−73 Reagents. Formic acid. Specifications

GOST 6835−2002 Gold and alloys on its basis. Brand

GOST 9147−80 Glassware and equipment lab porcelain. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

GOST 12026−76 laboratory filter Paper. Specifications

GOST 12338−81 Iridium powder. Specifications

GOST 12342−81 Rhodium powder. Specifications

GOST 12343−79 Ruthenium powder. Specifications

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 14919−83 electric Stoves, electric ovens and cabinets appliances. General technical requirements

GOST 18300−87 ethyl rectified technical. Specifications

GOST 25086−2011 non-ferrous metals and their alloys. General requirements for methods of analysis

GOST 25336−82 Glassware and equipment laboratory glass. The types, basic parameters and dimensions

GOST 29169−91 oils. Pipette with one mark

GOST 29227−91 oils. Pipettes are graduated. Part 1. General requirements

GOST 31290−2005 Platinum affilirovannaja. Specifications

GOST 31291−2005 Palladium refined. Specifications

GOST R 52501−2005 Water for laboratory analysis. Specifications

GOST R 52599−2006 Precious metals and their alloys. General requirements for methods of analysis

GOST R 53198−2008 Ores and concentrates of non-ferrous metals. General requirements for methods of analysis

GOST R 53228−2008 Scales non-automatic actions. Part 1. Metrological and technical requirements. Test

ST SEV 543−77 Number. Record rules and rounding

Note — When using this standard appropriate to test the effect of reference standards in the information system of General use — on the official website of the Federal Agency for technical regulation and Metrology on the Internet or in the annual information index «National standards» published as on January 1 of the current year, and the editions of the monthly information index «National standards» for the current year. If replaced with a reference standard, which was given an undated reference, then it is recommended to use the current version of this standard, taking into account all enabled in this version modifications. If replaced with a reference standard, which is given a dated reference, it is recommended to use the version of this standard referred to above by year of approval (acceptance). If after approval of this standard in the reference standard, which is given a dated reference, a change affecting a provision to which reference, the provision is recommended to be applied without taking into account this change. If the reference standard is cancelled without replacement, the position in which reference is made to him, recommended to be used in part not affecting this link.

3 General requirements

3.1 Methods of quantitative chemical analysis used in the control of the composition of non-ferrous metals and precious metals content must comply with the requirements of GOST R 8.563, GOST R ISO 5725−1, GOST R ISO 5725−2, GOST R ISO 5725−3, GOST R ISO 5725−4, GOST R ISO 5725−5, GOST R ISO 5725−6, 53198 GOST R and GOST R 52599 ensuring safety requirements according to GOST 12.0.001, GOST 12.0.003, GOST 12.0.004 and GOST 12.3.002.

Requirements to selection and preparation of samples for analysis regulated by the normative documents approved in the prescribed manner.

3.2 General requirements for measurements shall meet the requirements of GOST R 52599, GOST R and GOST 53198 25086.

3.2.1 For the analysis of used volumetric laboratory glassware according GOST 1770, pipettes according to GOST and GOST 29169 29227, glassware GOST 25336, porcelain crucibles according to GOST 9147.

3.2.2 reagents Used should have the qualification of «chemically pure» (hç), or «extra pure» (OS.CH.).

3.2.3 preparation Conditions, use and storage of solutions-defined components of known concentration, and duration of storage — by GOST 4212.

3.3 Analysis of samples of sulphide copper-Nickel ores of the precious metals conduct of the two definitions in terms of intermediate precision.

3.4 Monitoring of indicators of quality of measurement results is carried out using standard samples according to GOST 8.315.

3.5 When assessing the admissibility of the results of measurements using the recommendations of GOST R ISO 5725−6.

3.6 Analytical linkage matte and the volume of the analyzed solution is selected depending on the expected concentration detectable component in the sample.

3.7 the value of the result of the analysis should be terminated with a figure the same category as the value of the expanded uncertainty specified in table 3.

3.8 Rules for rounding of numbers shall conform to the requirements of ST CMEA 543.

4 safety Requirements

4.1 All works should be carried out with use of devices and installations, relevant regulations for electrical [1] and requirements of GOST 12.2.007.0.

4.2 When the equipment and installations required to comply with the requirements of GOST 12.3.019, GOST R 12.1.019 and [2], [3].

4.3 All equipment and installations should be equipped with devices for grounding in accordance with the requirements of GOST 12.2.007.0 and GOST 12.1.030. Grounding must conform to the rules of electrical devices [1].

4.4 Analysis carried out in rooms equipped with General dilution ventilation system according to GOST 12.4.021.

4.5 Monitoring of hazardous substances in the workplace air should be carried out in accordance with the requirements of GOST 12.1.007, GOST 12.1.005, GOST and GOST 12.1.014 12.1.016.

4.6 Organization of training of the working personnel to the requirements of labour safety — according to GOST 12.0.004.

4.7 the premises of the laboratory must comply with the fire safety requirements according to GOST 12.1.004 and have a extinguishing media in accordance with GOST 12.4.009.

4.8 laboratory Personnel must be provided with premises according to sanitary norms [4] for the group the production processes of IlIa.

4.9 laboratory Personnel must be provided with overalls, special footwear and other individual protection means, according to established norms [5].

5 Method of analysis

5.1 Method of mass spectrometric analysis

Mass-spectrometric method based on measurement of the intensity of the flow of ions, separated by mass-to-charge. As the ion source using inductively bound plasma, through which the spray enters the spray system of the measured solution. The dependence of the intensity divided by the ratio of the mass-to-charge flow of ions from the mass concentration of the components in the solution is established by means of calibration curve.

To ensure the representativeness of the analytical sample samples and lower detection limits of the content of precious metals carried out a preliminary collectormania precious metals Nickel matte with subsequent chemical sample preparation.

5.2 Preliminary collectormania precious metals in Nickel matte

The method is based on crucible smelting of the charge (mixture of analytical sample of the sample with fluxes), in which the formation of two stratified phases: slag (oxide) and matte (sulphide). Last quantitatively collective precious metals.

The mixture includes as a low-melting flux is anhydrous sodium tetraborate (anhydrous borax) and the estimated amount of Nickel sulfide or Nickel oxide with elemental sulfur as component steinbruchweg.

Anhydrous borax in the smelting process in itself dissolves rock-forming sample components (oxides of the elements) and formed in the process of melting the iron oxide, thus providing a full «autopsy» of sample material.

Nickel sulfide added to the charge or the resulting during the smelting process in the interaction of Nickel oxide with iron sulfide samples and (or) elemental sulfur dissolves in precious metals and base metal sulfides samples.

6 measurement Means, auxiliary devices, materials, reagents, solutions

The mass spectrometer of the Corporation «Thermo», model «X series 2» inductively coupled plasma.

Melting laboratory furnace providing heating temperature up to 1250 °C.

The thermoelectric Converter of the type TPP/1−0679 designed to measure temperature in the melting furnace, operating range 0 °C to 1300 °C.

Scale special accuracy class according to GOST R 53228. The required weighing accuracy is determined by the order of the task numbers weight the standard.

A vibrating type mill HSM 250-R.

A vibrating type mill «Pulverisette 9».

The mill rod.

Eraser disk type «Pulverisette 13».

Eraser disk type «Pulverisette 16».

A refractory crucible with a capacity of 500 cm.

Mold crucible metal.

Glass bottle with a glass lid.

Tongs, metal, chamotte crucibles.

Anvil.

Hammer.

File.

Anhydrous borax. For use in the assay collectormania, if necessary, gospelchor in a rod mill for 30 min.

Nickel oxide black GOST 4331.

Nickel powder according to GOST 9722.

Sulfur elemental «OS.h.» [6]. Before use are ground in two stages: the first is disk eraser type «Pulverisette 16» (large chopping); the second is disk eraser type «Pulverisette 13» (fine grinding).
________________
* POS.[6]-[13], see Bibliography. — Note the manufacturer’s database.


The Nickel sulfide.

Laboratory filter paper according to GOST 12026. Used for the manufacture of paper bags, which are sleep prepare the charge.

Cotton wool GOST 5679.

The technical rectified ethyl alcohol according to GOST 18300.

The consumption of alcohol on a clean mortar mixer mill when grinding the matte one sample is 1 cm.

Resistance furnace electric laboratory chamber type SNOL-1.6 and 2.5.1/9-М2У4.2, ensuring the heating temperature up to 1400 °C.

The electric oven according to GOST 14919, installed in a fume hood.

Crucibles TF-40-PORT, 16 CH GOST 25336.

Fiberglass filter.

Crucibles lundbye N 56, N 57 at [7].

Filters obestochennye «blue ribbon» at [8].

Nitric acid according to GOST 4461, 1 mol/DMequivalent.

Nitric acid is the OS.h. according to GOST 11125.

Hydrochloric acid OS.h. according to GOST 14261, diluted 1:1, 1:5, 1:99.

A mixture of hydrochloric and nitric acids in the ratio 3:1, freshly prepared.

Sulfuric acid according to GOST 4204, diluted 1:5.

Formic acid according to GOST 5848.

Water according to GOST R 52501 (deionized).

Barium peroxide [9].

Gold GOST 6835.

Platinum affilirovannaja according to GOST 31290.

Palladium refined according to GOST 31291.

Rhodium powder according to GOST 12342.

Ruthenium powder according to GOST 12343.

Iridium powder according to GOST 12338.

Thallium nitrate [10].

Cesium nitrate [11].

Tellurium [12].

A solution of 10 mg tellurium/cm.

Tin dichloride in [13].

A solution of tin dichloride, 0.1 g/cm.

Argon gas of the highest grade according to GOST 10157.

Volumetric flasks 2−25−2, 2−50−2, 2−100−2, 2−200−2, 2−250−2, 2−500−2, 2−2000−2 according to GOST 1770.

Cover of porcelain by GOST 9147.

Glass sticks with a length of 200−300 mm according to GOST 1770.

Pipettes 2−2-1, 2−2-2, 2−2-5, 2−2-10, 2−2-20, 2−2-25, 2−2-50 according to GOST 29169.

Pipette 1−1-2−1, 1−1-2−2, 1−2-2−5, 1−2-2−10 according to GOST 29227.

The glasses are In 1−100 TS-1-TS 200, 1−400 CU In-1−400 CU In-1−800 TS-1−1000 TS-1−2000 TC GOST 25336.

Crucible high 4 according to GOST 9147.

Cylinders 1−5-2, 1−10−2, 1−25−2, 1−100−2, 1−250−2, 1−1000−2 according to GOST 1770.

Funnel polypropylene.

Probyvala polypropylene.

Beakers capacity 50, 100, 250 cmaccording to GOST 1770.

Desiccator, according to GOST 25336.

Standard samples of composition of copper-Nickel sulfide ores, approved in the established order, for example, 8770−2006 GSO, GSO 8772−2006, 8773−2006 GSO, GSO 8774−2006.

Note — it is permitted to use other measurement means, auxiliary devices, glassware, chemical reagents and materials, providing the metrological characteristics, in accordance with the requirements of this standard.

7 Preparing for measurement

7.1 Obtaining Nickel sulfide

Method 1

100,0 g of Nickel oxide, 50.0 g of elemental sulfur and 80,0 g of borax mixed in a glass jar. The resulting mixture was poured into a paper bag. The bag with the mixture placed in a pre-heated to the operating temperature of the refractory crucible and put into the melting furnace. Melting is carried out at a temperature from 1100 °C to 1250 °C for 45 min.

The melt is poured into a metal crucible and the mold is cooled for 30 min. the Mold with the cooled melt upset on the anvil and beat with a hammer the slag from the sulphide of Nickel (matte). Matte break into pieces and ground in a vibratory mill for 10 to 20 seconds.

Method 2

70,0 g of Nickel powder, 35,0 g of sulfur elemental and 80.0 g of anhydrous borax mixed in a glass jar. The resulting mixture was poured into a paper bag. Further according to method 1 with the words «the bag with the mixture… «.

7.2 Preparation of solutions of tellurium in 10 mg/cm

A portion of the elemental tellurium of 20.00 g is placed in a beaker with a capacity of 2000 cm, is dissolved in an amount of from 150 to 200 cmmixture of hydrochloric and nitric acids (3:1), evaporated to a volume of 3 to 5 cm, flow 20 cmof hydrochloric acid and again evaporated to a volume of 3 to 5 cm. The operation is repeated three times. Pour 20 cmof hydrochloric acid and transferred to volumetric flask with a capacity of 2000 cm, priliva hydrochloric acid to a total volume of from 1550 to 1600 cm. Topped up to the mark with water.

7.3 preparation of the solution of tin dichloride 0.1 g/cm

A portion of tin dichloride of 100.00 g were placed in a glass with a capacity of 1000 cm, flow 250 cmof hydrochloric acid, dissolved by heating, cooled, made up to 1000 cmof water, stirred with a glass rod and filtered through filter «blue ribbon».

7.4 Preparation of the mass spectrometer measurements

7.4.1 switching on and preparation of the mass spectrometer to carry out work in accordance with the manual.

7.4.2 When performing measurements using isotopes of the designated component and the components of the comparison according to table 1.


Table 1 — Isotopes-defined components and components comparisons

The name of the designated component	Isotope-defined component.e.m.	The component name comparison	Isotope component comparison, and.e.m.
Platinum	195	Thallium	205
Palladium	108	Cesium	133
Rhodium	103	Cesium	133
Ruthenium	101	Cesium	133
Iridium	191	Thallium	205
Gold	197	Thallium	205

7.4.3 During the measurements comply with the following conditions:

— output power, W	1100−1350
— cooling argon flow, DM/min	13−15
— the speed of the additional argon flow, DM/min	0,7−1,5
— the speed of the conveying argon flow, DM/min	0,6−0,9
— the rotation speed of the peristaltic pump, rpm	70−100
— pressure of argon is applied to the input of the gas system, MPa	0,5−0,7
— the integration time of a single isotope, with	2,0
— measurement mode	relative
the number of measurements of analytical signal	3
— submission of solution component comparison, the spray system produced by a separate capillary.

The optimum voltage setting on the detector settings of the ion optics and position of the burner is carried out automatically in accordance with the user manual.

Allowed to use other components as a component comparison, other measurement conditions, providing the satisfactory results of the eligibility check in accordance with section 11 and control of accuracy of measurement in accordance with section 12.

7.5 Preparation of one-component solutions of known concentration

7.5.1 the platinum Solution

Solution A

A portion of platinum 5,0000 g placed in a beaker with a capacity of 1000 cm, 70−100 cm pour themixture of hydrochloric and nitric acids (3:1), with a lid and heated until complete dissolution of the sample. The solution was evaporated to small volume, poured 5−7 cmof hydrochloric acid, again evaporated to a small volume. The operation is repeated three or four times. Pour the 20−30 cmof hydrochloric acid and transferred the solution into a volumetric flask with a capacity of 500 cmwith hydrochloric acid (1:1). In the glass, which had a dissolution, poured 20−50 cmof hydrochloric acid (1:1), bring to a boil under the same cover, cooled and transferred into the same volumetric flask. The operation is repeated two or three times. Topped up to the mark with the same acid.

1 cmof solution A contains 10 mg of platinum.

Solution A. 1

In a volumetric flask with a capacity of 100 cmis placed 20 cmof solution A, made up to the mark with hydrochloric acid (1:1). From the resulting solution take aliquot part 5 cm, placed in a flask with a capacity of 100 cm, made up to the mark with hydrochloric acid (1:1).

1 seesolution A. 1 contains 100 µg of platinum.

7.5.2 Solution of palladium

Solution A

A portion of palladium 5,0000 g placed in a beaker with a capacity of 1000 cm, moistened with 3−5 cmof formic acid, dried on the stove and dissolve under the hood in the 80−100 cmof a mixture of hydrochloric and nitric acids (3:1), gradually Prilepa her portions at 20−30 cm.

The solution was evaporated to a small volume. Cooled, poured 5−7 cmof hydrochloric acid, again evaporated to a small volume. The operation is repeated three or four times. Pour the 20−30 cmof hydrochloric acid, dissolve the salt when it is heated, not boiling. The solution was cooled, transferred to a volumetric flask with a capacity of 500 cmwith hydrochloric acid (1:1). In a glass, in which were a dissolution, poured 20−50 cmof hydrochloric acid (1:1), bring to a boil under the same cover, cooled and transferred into the same volumetric flask. The operation is repeated two or three times. Topped up to the mark with the same acid.

1 cmof solution A contains 10 mg of palladium.

Solution A. 1

In a volumetric flask with a capacity of 100 cmis placed 20 cmof solution A, made up to the mark with hydrochloric acid (1:1). From the resulting solution take aliquot part 5 cm, placed in a flask with a capacity of 100 cm, made up to the mark with hydrochloric acid (1:1).

1 seesolution A. 1 contains 100 µg of palladium.

7.5.3 Solution of rhodium (iridium, ruthenium)

Solution A

A portion of the rhodium (iridium, ruthenium) 0,5000 g Lundby placed in the crucible, ground with a glass rod with a 2.5−3.0 g of peroxide of barium. The crucible is placed in a cold furnace, heated to a temperature of 900 °C, incubated for 2 h, cooled in furnace. The sintering crucible placed in a beaker with a capacity of 800−1000 cm, cover with a lid, pour the portions under the cover of hydrochloric acid (1:1) to the upper edge of the crucible and heated to dissolve the cake.

The crucible is removed from the glass, carefully washed over a glass of hydrochloric acid (1:1) was placed in a beaker with a capacity of 200 cm, go to the top of the crucible with hydrochloric acid (1:1), bring to the boil and the solution attach to the core. Operation steaming Cup repeat two to three times, dried on a hot plate, cooled and placed in desiccators.

The combined solution is evaporated under the hood to a volume of 100−120 cm, filtered into a glass with a capacity of 2,000 cmusing two of the filter «blue ribbon», washed filters five or six times with hydrochloric acid (1:5) (before the disappearance of the pink coloration of the filter).

Filter Lundby placed in a crucible placed in a furnace, heated to temperature 600−650 °C, cooled, removed from the oven, add 0.5−1.5 g of peroxide of barium, an operation of sintering and dissolution of SPECA repeat three to five times (to eliminate dark inclusions plus control sintering).

The combined filtrate was evaporated under the hood 30−50 cm, 10−20 cm pouredhydrochloric acid, the volume was adjusted to 1000 cmwater is heated. Slowly pour portions of 10−30 cmhot sulphuric acid (1:5), while stirring with a glass rod until complete precipitation of the barium sulphate, avoiding excess of sulfuric acid. Complete precipitation of the barium sulfate test, priliva on the side of a glass drops of sulfuric acid (1:5). Solution and the precipitate leave in a warm place for 1−2 hours (no more than two hours), filtered through two filter «blue ribbon» in a glass with a capacity of 2,000 cm, the filter was washed 10−15 times with hydrochloric acid (1:99).

The filtrate is evaporated to a volume of 30−50 cm, transfer with hydrochloric acid (1:1) in a volumetric flask with a capacity of 250 cm. In a glass, in which were a dissolution, poured 20−25 cmof hydrochloric acid (1:1), bring to a boil under the same cover, cooled and transferred into the same volumetric flask. The operation is repeated two or three times. Topped up to the mark with the same acid.

1 cmof the solution contains 2 mg of rhodium (iridium, ruthenium).

Solution A. 1

In a volumetric flask with a capacity of 100 cmis placed 5 cmof solution A, made up to the mark with hydrochloric acid (1:1).

1 seesolution A. 1 contains 100 µg of rhodium (iridium, ruthenium).

A solution of rhodium (ruthenium)

In a volumetric flask with a capacity of 100 cmare placed 50 cmof A solution of rhodium (ruthenium), made up to the mark with hydrochloric acid (1:1).

1 cmof the solution contains 1 mg of rhodium (ruthenium).

The solution of iridium

In a volumetric flask with a capacity of 100 cmis placed 25 cmof the solution And iridium, made up to the mark with hydrochloric acid (1:1).

1 cmof the solution contains 500 µg of iridium.

7.5.4 Solution of gold

Solution A

A portion of the gold 1,0000 g placed in a beaker with a capacity of 800 cm, 50−70 cm, pour themixture of hydrochloric and nitric acids (3:1), covered with a lid, heated to dissolve the sample, evaporated to a small volume.

Pour 2−3 cmof hydrochloric acid, evaporated to a small volume. This operation is repeated two or three times. Pour 0.5−1.0 cmof nitric acid and 10−12 cmof hydrochloric acid, transferred into a volumetric flask with a capacity of 500 cmwith hydrochloric acid (1:1). In the glass, which had a dissolution, poured 20−50 cmof hydrochloric acid (1:1) and 2−3 drops of nitric acid, boil for 5−7 min under the same cover, cooled and transferred into the same volumetric flask. The operation is repeated two or three times. Topped up to the mark with the same acid.

1 cmof the solution contains 2 mg of gold.

Solution A. 1

In a volumetric flask with a capacity of 200 cmis placed 10 cmsolution A, made up to the mark with hydrochloric acid (1:1).

1 seesolution A. 1 contains 100 micrograms of gold.

Solution B

In a volumetric flask with a capacity of 100 cmare placed 50 cmof the solution And of gold, made up to the mark with hydrochloric acid (1:1).

1 cmof the solution contains 1 mg of gold.

7.5.5 Solution of thallium

A portion of nitrate of thallium 0,130 g placed in a beaker with a capacity of 100 cm, is dissolved in 10−12 cmof nitric acid 1 mol/DMequivalent, transferred to a volumetric flask with a capacity of 100 cmand then filled to the mark with the same acid.

1 cmof the solution contains 1 mg of thallium.

7.5.6 Solution of cesium

The weight of cesium nitrate 0,147 g placed in a beaker with a capacity of 100 cm, dissolved in 10−15 cmof nitric acid 1 mol/DMequivalent, transferred to a volumetric flask with a capacity of 100 cmand then filled to the mark with the same acid.

1 cmof the solution contains 1 mg of cesium.

7.6 Preparation of multi-component solutions of known concentration

The Solution I

In a volumetric flask with a capacity of 200 cmis placed 10 cmsolution And platinum, 40 cmof A solution of palladium, 20 cmof a solution of rhodium, 10 cmsolution And gold 10 cmof a solution of ruthenium, 4 cmof a solution of iridium, made up to the mark with hydrochloric acid (1:1).

1 cmof solution I contains 500 micrograms of platinum, palladium 2000 µg, 100 µg of rhodium and gold, with 50 g of ruthenium, 10 µg of iridium.

Solution II

In a volumetric flask with a capacity of 100 cmis placed 5 cmof solution I, made up to the mark with hydrochloric acid (1:1).

1 cmof solution II contains 25 micrograms of platinum, 100 g of palladium, 5 g of rhodium and gold, 2.5 ág of ruthenium, 0.5 µg of iridium.

Solution III

In a volumetric flask with a capacity of 100 cmis placed 5 cmof solution II, made up to the mark with hydrochloric acid (1:1).

1 cmof solution III contains a 1.25 micrograms of platinum, palladium 5 µg, 0.25 µg of rhodium and gold of 0.125 µg of ruthenium, iridium of 0.025 µg.

Solution IV

In a volumetric flask with a capacity of 100 cmis placed 5 cmA. 1 solutions of platinum, palladium, rhodium, ruthenium, iridium and gold, made up to the mark with hydrochloric acid (1:1).

1 cmof the IV solution contains 5 micrograms of platinum, palladium, rhodium, ruthenium, iridium, gold.

7.7 Preparation of solutions internal standard to measure by a mass spectrometer

Solution la

In a volumetric flask with a capacity of 100 cmis placed 20 cmof a solution of cesium and 20 cmof a solution of thallium, made up to the mark with hydrochloric acid (1:5).

1 cmof the la solution contains 0.2 mg of cesium and thallium.

A Solution Of IIa

In a volumetric flask with a capacity of 100 cmis placed 2 cmla solution, made up to the mark with hydrochloric acid (1:5).

1 cm of solution IIa contains 4 micrograms of cesium and thallium.

A Solution Of IlIa

In a volumetric flask with a capacity of 500 cmis placed 6 cmof solution IIa, made up to the mark with hydrochloric acid (1:5).

1 cmof solution IlIa contains 48 ng of cesium and thallium.

7.8 Preparation of the calibration solutions

When preparing solutions using hydrochloric acid OS.h. and deionized water.

The mass concentration of components in the calibration solutions are presented in table 2.


Table 2 — Mass fractions of the components in the calibration solutions

Room calibration solution	Mass concentration of the component, ng/cm
	Platinum	Palladium	Rhodium	Ruthenium	Iridium	Gold
1	125	500	25	12,5	2,5	25
2	50	200	10	5,0	1,0	10

Solution 1

In a volumetric flask with a capacity of 100 cmis placed 10 cmsolution III and 20 cmdeionised water, made up to the mark with hydrochloric acid (1:5).

Solution 2

In a volumetric flask with a capacity of 100 cmis placed 4 cmof solution III and 8 cmdeionised water, made up to the mark with hydrochloric acid (1:5).

Calibration solutions used in the preparation day.

7.9 Solutions to check the correctness of measurement results

Solution 3

In a volumetric flask with a capacity of 100 cmis placed 2 cmof IV solution, made up to the mark with hydrochloric acid (1:5).

1 cm3 of solution contains 100 ng of platinum, palladium, rhodium, ruthenium, iridium, gold.

A solution of 4

In a volumetric flask with a capacity of 100 cmplaced 1 cmIV solution, made up to the mark with hydrochloric acid (1:5).

1 cmof the solution 4 contains 50 ng of platinum, palladium, rhodium, ruthenium, iridium, gold.

A solution of 5

In a volumetric flask with a capacity of 100 cmis placed 10 cm3 of a solution, made up to the mark with hydrochloric acid (1:5).

1 cmof the solution contains 5 to 10 ng of platinum, palladium, rhodium, ruthenium, iridium, gold.

A solution of 6

In a volumetric flask with a capacity of 100 cmis placed 5 cm3 of solution, made up to the mark with hydrochloric acid (1:5).

1 cmsolution 6 contains 5 ng of platinum, palladium, rhodium, ruthenium, iridium, gold.

The solutions used in the preparation day.

7.10 Construction of calibration characteristics

7.10.1 the Calibration of the mass spectrometer is carried out before the beginning of measurements of the series of samples prepared in accordance with the user instruction under the conditions according to 7.4.3.

Note — a Series — a set of samples to analyse in the course of the working day.


For construction of calibration characteristics using a background solution of hydrochloric acid (1:5) and the calibration solutions, prepared according to 7.8, in order of increasing mass concentrations of the identified components. The dependence of the relative intensities of the separated ion flow isotope-defined component to the flux intensity of the internal standard from the mass concentration is set using the software. For calibration and measurement using a solution of internal standard IlIa.

The relative standard deviation RSD of the analytical signal for each of the designated component must be less than 3%, the correlation coefficient is not less than 0,999.

After the construction of the calibration characteristics is carried out a control operation 12.1.

8 performance measurement

8.1 Calculation of the charge

The burden calculation is carried out based on the content in the alloy of Nickel, copper and sulfur. The composition of the charge includes: a charge of analytical samples of the test material, the drill and, if necessary, the oxide or the sulfide Nickel, elemental sulfur.

Depending on the mass fraction of sulfur in the test sample choose a method of producing a collector. When the mass fraction of sulfur no more than 7.5%, choose the option of receiving collector # 1, more than 7.5% — N 2 option.

Estimated weight matte should be from 10 g to 30 g and contain at least 10% by weight of the slag.

8.1.1 Option 1 N

The calculation of the charge composition is performed on a portion of analytical samples weighing 50 g.
________________
If the sample mass less than 50 g, further calculation is performed on available sample mass.


When crucible melting as a result of thermal dissociation of sulphide minerals from the material sample the sample is formed matte own sulphides. Reactions thermal dissociation is given below:

chalcopyrite
pentlandite
pyrrhotite

8.1.1.1 calculation of the mass of matte from own sulfides, members of the sample material

The calculation is carried out in the following sequence:

a) calculation of the sulphides of Nickel and copper from the sample material

Mass of copper sulfide from a sample of sample , g

, (1)

where  — mass fraction of copper in the sample, %;

 — analytical linkage of sample, g;

1.25 conversion ratio of copper in the copper sulfide (I).

The mass of Nickel sulfide from a sample of sample , g

, (2)

where  — mass fraction of Nickel in the sample, %;

1,36 — conversion rate of Nickel to Nickel sulfide composition heazlewoodite ().

b) calculation of residual sulfide sulfur from the sulfides of copper and Nickel from the analytical sample of the sample (point a), , g

, (3)

where  — mass fraction of sulfur in the sample, %;

1,50 — conversion rate of copper at higher copper sulfide ();

1.55 V is the ratio of Nickel to higher Nickel sulfide ().

C) calculate the mass of iron sulfide (II), Stein, a , g

, (4)

where is 2.74, the ratio of the residual sulfur in the iron sulfide (II).

g) calculate the mass of matte from native sulphides of copper, Nickel and iron from the material of the analytical sample , g

. (5)

8.1.1.2 calculate the mass of anhydrous borax in the charge

Calculate the mass of the analytical portion of the sample, resulting in the melting crucible resulted in the slag g, by the formula

, (6)

where 1,57 — the ratio of iron sulfide (II) to iron.

Weight of anhydrous borax , introduced into the composition of the batch must exceed three times with rounding up the number .

. (7)

8.1.1.3 calculation of the mass of the Nickel sulfide obtained according to 7.1 (method 1 or 2) in the charge.

Estimated weight of the manifold must be not less than 10% by weight of the slag. A lot of dross , g, is calculated by the formula

. (8)

The mass of Nickel sulfide introduced into the composition of the charge , g, is calculated by the formula with rounding up to whole

. (9)

8.1.2 Option 2 N

When the mass fraction of sulfur in the sample of the test material more than 7.5% of Nickel in the matte as the result of melting crucible formed insoluble in hydrochloric acid iron-Nickel alloys, which prevents further mass spectrometric determination of precious metal content. To prevent the formation of iron-Nickel alloys iron from the analytical sample with melting crucible in the form of oxides is transferred to the slag. As the oxidizing agent the composition of the batch enter the estimated amount of Nickel oxide.

In the first stage of the calculation determines the maximum analytical sample, taking into account two limitations:

1. Mass fraction of copper in the calculation of the matte should not exceed 14%. Otherwise, after the dissolution of matte in hydrochloric acid in the insoluble residue, there is an increased copper content, further complicating the measurement of precious metal content on a mass spectrometer.

2. Calculations performed on Nickel matte composition heazlewoodite () with a sulfur mass fraction of 26.7%. Excess sulfur leads to a higher content of iron sulfide in the matte, which also affects the dissolution process.

The maximum possible mass of analytical sample of the sample from the mass fraction of copper , g, is calculated by the formula

, (10)

where is the specified weight of the matte,
________________
It is recommended that 20 g.


The maximum possible mass of analytical sample samples from the sulphur mass fraction , g, is calculated by the formula

. (11)

If and more than 50 grams, a further calculation is performed on a portion of the sample weighing 50 g. If one out of a maximum possible mass, or both at least 50 g, further calculation is carried out on a smaller mass rounded to the nearest of a number .

. (12)

For oslavany contained in the weighed sample of the test material in the form of iron sulphides required in the composition of the charge to impose a Nickel oxide. Mass of Nickel oxide , g, is calculated by the formula

, (13)

where is the mass of iron sulfide material sample sample calculated by the formula (4);

1.15 — coefficient equal to the weight of Nickel oxide, g for the oxidation of 1 g of iron sulfide.

A lot of matte formed from sulfatirovnie of Nickel oxide with iron sulphide , g, is calculated by the formula

, (14)

where to 1.07 — the ratio of Nickel oxide to Nickel sulfide ().

A lot of Stein , g, from the native sulphides of copper and Nickel from the analytical sample of the sample (formula 1−2) and of Nickel sulfide from Nickel oxide (formula 14) is calculated by the formula

. (15)

If , in the charge composition additionally introduced Nickel oxide and sulfur elemental.

A lot of additional Nickel oxide , g, is calculated by the formula

. (16)

Thus, the mass of the Nickel oxide , and elemental sulfur , g, in the charge calculated by the formulas

, (17)

, (18)

where the 0.50 is the coefficient numerically equal to the mass of elemental sulfur, g, required to sulfatirovnie 1 g of Nickel oxide.

Weight of anhydrous borax , introduced into the composition of the batch must exceed three times the weight of the portion of the sample with rounding up the number .

8.2 Preparation of the charge and crucible melting

According to the results of the calculations (for 8.1) the components of the batch weigh: analytical weighed to the nearest 0.01 g borax to 1 g and, optionally, a sulfide or Nickel oxide and sulfur element — 0.1 g, poured into a glass jar that is closed with the lid and stirred the contents for 1 min. pour Contents of the jar in a paper bag.

A package of charge is placed in the heated to operating temperature fireclay crucible tongs and put into the melting furnace. Melting is carried out at a temperature of from 1100 to 1200 °C for 1 h. after melting, the melt from the crucible is poured into a metal mold and leave for 20−25 minutes to cool. Then extract the contents of the mold and on the anvil with a hammer striking the slag from the matte. The remaining particles of slag on the matte removed with a file.

The prepared matte is weighed with accuracy to the second decimal point and milled in a vibrating mill for 3−5 sec (mixer mill type HSM-250-R) and 3−10 (for the type of mill «Pulverisette 9»). Pour the resulting powder in a porcelain crucible. Picked batch of matte is passed to the subsequent stages of chemical sample preparation.

Headset vibration grinding mill after crushing process clean wool (or shop towels) moistened with alcohol. Upon completion of the grinding mills vibrating headset is washed with soap solution and dried.

Likewise, the second analytical linkage, performing further operations 8.3 and 8.4 with each of the analytical batches.

8.3 Chemical sample preparation

A portion of the matte with a mass of 3.00 g or 5.00 g is placed in a beaker with a capacity of 400 cm, moistened with water, poured from 150 to 180 cmof hydrochloric acid, dissolve by heating under a lid, not allowing to boil, until the termination of allocation of hydrogen sulfide.

Pour 1 cmof a solution of tellurium and leave in a warm place for 20−25 minutes then pour 5 cmof a solution of dichloride of tin, stand for coagulation of sludge for another 10−15 min (until clarification of the solution).

The resulting precipitate was filtered off through the filter crucible. The beaker and the residue on the filter is washed five or six times with hot water.

The crucible is placed in a beaker, which was carried out dissolution, and poured 50−100 cmof a mixture of hydrochloric and nitric acids (3:1), incubated 30 min. the Glass is transferred to a warm plate and continue the digestion for 30−60 min.

A glass rod take out a crucible from a glass, wash it two or three times with water, the porous bottom of the crucible is washed under pressure. The solution was evaporated to a volume of 5−10 cm, priliva two or three times 1−2 cmof hydrochloric acid.

The solution was transferred to volumetric flask with a capacity of 25−100 cm, pour 3−5 drops of nitric acid and then filled to the mark with hydrochloric acid (1:5).

Depending on the intended mass concentration of the components in the solution, carry out its corresponding dilution. In this case the expected mass concentration of the determined components in the sample solution should be less than 0.1 ng/cm.

The total salt composition of the analyzed solution should not exceed 2 mg/cmin accordance with the manual of the device.

8.4 measurements on the mass spectrometer

The measurement of mass concentration of the components is carried out after preparation of the mass spectrometer to work in accordance with 7.4, the calibration and control 12.1. The relative standard deviation RSD of the analytical signal for each of the designated component must be less than 3%. The measurement results are automatically stored in the database in electronic form. For later calculations we use the arithmetic average of the three analytic signals satisfying the above condition.

9 considering the contribution of the «single» experience

If the composition of the batch is added to the sulphide of Nickel, it is necessary to consider the contribution of «idle» experience in the measurement result.

9.1 calculation of the contribution of «idle» experience with the addition of Nickel sulfide

From the obtained according to 7.1 of Nickel sulfide from a batch of Nickel oxide (method 1) or Nickel powder (method 2) select five batches weighing 5.00 grams, then 8.3 conduct chemical training. The solution from each sample was transferred to volumetric flask with a capacity of 25 cm. Further in 8.4 complete the measurement of the concentrations of the identified components in the solution and converted to the mass share of Nickel sulfide , g/t, according to the formula

, (19)

where is the mass concentration of the determined component in solution «blank» of the experience, ng/cm.

The contents of the designated components in the Nickel sulfide is calculated as the arithmetic mean value of five parallel measurements and distribute the whole Nickel sulfide obtained from the party the source of the reagent.

9.2 calculation of the contribution of «idle» experience with the addition of Nickel oxide

A portion of the Nickel oxide mass of 100 g, selected from the party of reactant, floated on 7.1, method 1. The matte is weighed, crushed, taken away five batches weighing 5.00 g, conduct chemical preparation of the sample to 8.3 with final solution volume of 25 cm. Further in 8.4 complete the measurement of the concentrations of the identified components in the solution and converted to the mass share of Nickel sulfide , g/t, according to the formula

, (20)

where is the mass of matte «single» experience on 7.1, method 1,

The contents of the designated components, calculated as the arithmetic mean value of five parallel measurements and distribute to the entire batch of the reagent.

The algorithm taking into account the contribution of «idle» experience is given in 10.2.

10 Processing of measurement results

10.1 Mass fraction of the designated component , g/t (definition of), calculated by the formula

, (21)

where is the mass concentration of the determined component in solution, ng/cm;

 — the mass of the analytical sample, g;

is the mass of Nickel in matte, g;

 — the suspension of Nickel matte, taken for analysis, g;

 — the volume of the analyzed solution, cm;

 — the dilution factor.

10.2 In the case of adding the composition of the batch of sulphide or Nickel oxide mass fraction of the designated component, net of the contribution of «idle» experience , g/t, calculated by the formula

, (22)

where  — mass fraction of the designated component, calculated according to the formula (21), g/t;

 — mass fraction of the designated component in the sulfide or Nickel oxide, of the formula (19), (20), respectively, g/t;

 — the mass of Nickel sulfide, is added to the mixture, the formula (9), g;

 — the mass of the Nickel oxide added to the mixture, the formula (17), g;

 — the mass of the analytical sample,

11 Checking the admissibility of the results of measurements obtained under conditions of intermediate precision

The measurement result should be the arithmetic mean value of the results of the two determinations and is obtained under conditions of intermediate precision with the following condition

, (23)

where is the limit of intermediate precision, the values of which are given in table 3.


Table 3 — Ranges of the mass fraction of the designated component value of the standards intermediate precision, reproducibility, and accuracy rate — the expanded uncertainty of the measurement results of samples of ores sulphide copper-Nickel

In grams per ton

The name and range of mass fraction of the designated component					Indicator intermediate accurate precise- Onesti (average quadrati- as the deviation of the prom- intermediate kin- zivnosti)	Limit intermediate accurate precise- Onesti (for the results of the two determination income) if	The limit of rehabilitation of conductivity (for two measurements made in different laboratories) when	Extended the indefinite- laziness when
Platinum
From 0,0050 0,0100 to incl.					0,00072	0,0020	0,0024	0,0017
SV.	0,010	«	0,020	«	0,0014	0,004	0,005	0,004
«	0,020	«	0,050	«	0,0032	0,009	0,011	0,008
«	0,050	«	0,100	«	0,0069	0,019	0,023	0,016
«	0,100	«	0,200	«	0,012	0,033	0,040	0,028
«	0,20	«	0,50	«	0,022	0,06	0,07	0,05
«	0,50	«	Of 1.00	«	0,040	0,11	0,13	0,09
«	Of 1.00	«	Of 2.00	«	0,072	0,20	0,24	0,17
«	2,0	«	5,0	«	0,14	0,4	0,5	0,4
«	5,0	«	10,0	«	0,29	0,8	1,0	0,7
«	10,0	«	20,0	«	0,47	1,3	1,6	1,1
«	20	«	50	«	0,9	3	4	3
«	50	«	100	«	2,2	6	9	6
«	100	«	200	«	3,6	10	14	10
Palladium
From 0.010 to 0.020 incl.					0,0014	0,004	0,005	0,004
SV.	0,020	«	0,050	«	0,0032	0,009	0,011	0,008
«	0,050	«	0,100	«	0,0065	0,018	0,022	0,016
«	0,100	«	0,200	«	0,013	0,035	0,042	0,030
«	0,20	«	0,50	«	0,025	0,07	0,10	0,07
«	0,50	«	Of 1.00	«	0,054	0,15	0,18	0,13
«	Of 1.00	«	Of 2.00	«	0,087	0,24	0,29	0,21
«	2,0	«	5,0	«	0,18	0,5	0,6	0,4
«	5,0	«	10,0	«	0,36	1,0	1,2	0,9
«	10,0	«	20,0	«	0,65	1,8	2,2	1,4
«	20	«	50	«	0,8	3	3	2
«	50	«	100	«	2,2	6	7	5
«	100	«	200	«	3,6	10	12	9
«	200	«	600	«	9,4	26	31	22
Rhodium
From 0,0010 to 0,0020 incl.					0,00029	0,0008	0,0010	0,0007
SV.	0,0020	«	0,0050	«	0,00051	0,0014	0,0015	0,0011
«	0,0050	«	0,0100	«	0,00079	0,0022	0,0026	0,0018
«	0,010	«	0,020	«	0,0014	0,004	0,004	0,003
«	0,020	«	0,050	«	0,0029	0,008	0,010	0,007
«	0,050	«	0,100	«	0,0043	0,012	0,014	0,010
«	0,100	«	0,200	«	0,0072	0,020	0,024	0,017
«	0,20	«	0,50	«	0,014	0,04	0,05	0,04
«	0,50	«	Of 1.00	«	0,025	0,07	0,08	0,06
«	Of 1.00	«	Of 2.00	«	0,051	0,14	0,17	0,12
«	2,0	«	5,0	«	0,11	0,3	0,4	0,3
Ruthenium
From 0,0010 to 0,0020 incl.					0,00032	0,0009	0,0011	0,0008
SV.	0,0020	«	0,0050		0,00058	0.0016 inch	0,0019	0,0013
«	0,0050	«	0,0100	«	0,00090	0,0025	0,0030	0,0021
«	0,010	«	0,020	«	0,0018	0,005	0,006	0,004
«	0,020	«	0,050	«	0,0032	0,009	0,011	0,008
«	0,050	«	0,100	«	0,0069	0,019	0,023	0,016
«	0,100	«	0,200	«	0,0130	0,036	0,043	0,031
«	0,20	«	0,50	«	0,029	0,08	0,10	0,07
«	0,50	«	Of 1.00	«	0,047	0,13	0,16	0,11
«	Of 1.00	«	Of 2.00	«	0,072	0,20	0,26	0,17
Iridium
From 0,0010 to 0,0020 incl.					0,00029	0,0008	0,0010	0,0007
SV.	0,0020	«	0,0050	«	0,00058	0.0016 inch	0,0019	0,0013
«	0,0050	«	0,0100	«	0,00087	0,0024	0,0029	0,0021
«	0,010	«	0,020	«	0,0014	0,004	0,005	0,004
«	0,020	«	0,050	«	0,0032	0,009	0,011	0,008
«	0,050	«	0,100	«	0,0054	0,015	0,018	0,013
«	0,100	«	0,200	«	0,0108	0,030	0,036	0,026
«	0,20	«	0,50	«	0,025	0,07	0,08	0,06
Gold
From 0,0020 0,0050 to incl.					0,00036	0,0010	0,0012	0,0009
SV.	0,0050	«	0,0100	«	0,00076	0,0021	0,0025	0,0018
«	0,010	«	0,020	«	0,0014	0,004	0,005	0,004
«	0,020	«	0,050	«	0,0029	0,008	0,010	0,007
«	0,050	«	0,100	«	0,0058	0,016	0,019	0,013
«	0,100	«	0,200	«	0,010	0,028	0,034	0,024
«	0,20	«	0,50	«	0,018	0,05	0,06	0,04
«	0,50	«	Of 1.00	«	0,036	0,10	0,12	0,09
«	Of 1.00	«	Of 2.00	«	0,072	0,20	0,24	0,17
«	2,0	«	5,0	«	0,14	0,4	0,5	0,4
«	5,0	«	10,0	«	0,25	0,7	0,8	0,6
«	10,0	«	20,0	«	0,51	1,4	1,7	1,2
«	20	«	50	«	1,1	3	4	3

If condition (23) is not satisfied, then get another result under conditions of intermediate precision.

Note — an Additional determination may be performed by one of the previously held operators.


If the discrepancy between the largest and smallest of the three result () is less than or equal to the value of the critical range , as a final result take an arithmetic average value of three result.

The critical range for the three results calculated according to the formula

, (24)

where 3,31 — ratio tabulated at confidence probability of 0.95 for the three outcomes definitions;

 — the standard deviation of intermediate precision, the values of which are given in table 3.

If the difference () is greater than the value of the critical range , then find out the causes of unacceptable results, definitions and eliminate them.

12 accuracy Control of measurement results

12.1 Control calibration characteristics

Control of the calibration characteristics is performed after calibration (before the beginning of measurements at 8.4), and after a series of 6−10 measurements from solutions of samples analysed.

To control the calibration characteristics using the solutions prepared at 7.9, to check the correctness of measurement results.

The control result is confirmed to be satisfactory when the condition

, (25)

where is the ratio control calibration characteristics, ng/cm;

 — played for the calibration characteristic value of the mass concentration of a specific component in the solution prepared according to 7.9 ng/cm;

 — assigned (reference) value of the mass concentration of a specific component in the solution at 7.9, ng/cm.

If the control of the calibration characteristics of the condition (25) is not satisfied, the results obtained in miscontrolling period, recognize unacceptable and perform a rebuild and check the calibration characteristics. Repeated failure of conditions (25) find out the reasons and eliminate them.

12.2 verification of measurements using the standard samples

Operational control of the correctness of the measurement carried out by analyzing a standard sample that meets the requirements of 3.4. When the analysis is performed in two definitions in terms of intermediate precision and check that the condition (23).

The result of the above procedures , g/t, calculated by the formula

, (26)

where the value of the mass fraction of the designated component in the standard sample, g/t, (the result of test measurements);

 — certified value of the mass fraction of the designated component in the standard sample, g/t.

The control result is confirmed to be satisfactory when the condition

, (27)

where  — norm of the control g/t.

At confidence probability of 0.95, the standard control is taken to equal the value of the expanded uncertainty given in table 3.

If the condition (27) control is repeated. Repeated failure conditions (27) find out the reasons of unsatisfactory results, and eliminate them.

12.3 Control of reproducibility of measurement results

Control of reproducibility is carried out in the event of disagreement between the two laboratories.

Measure the mass fraction of the designated component in the same sample in two laboratories. Calculate the absolute difference between the obtained measurement results and :

. (28)

The testing results confirmed to be satisfactory, if not exceed the limit of reproducibility , the values of which are given in table 3.

The standards of control precision, repeatability and increased control precision — the expanded uncertainty given in table 3.

13 Making measurements

The result of measuring the mass fraction of precious metals in the ore present as follows:

g/t,

where the value of the mass fraction of precious metals in the ore, g/t;

the value of the expanded uncertainty g/t.

14 Requirements for qualification

To perform analysis allowed persons over the age of 18, trained in the prescribed manner and allowed to work independently on used equipment.

Bibliography

[1] PUE	Regulations for electrical installation (PUE), as approved by the Ministry of energy of the Russian Federation, 1999, 7th edition
[2]	Rules of technical operation of electrical installations, approved by order No. 6 of the energy Ministry of the Russian Federation dated 13.01.2003
[3] POT RM-016−2001 RD 153−34.0−03.150−00	Interbranch rules on labor protection (safety rules for electrical installations approved by order of RF Ministry of energy dated 27.12.2000 No. 163 and the Resolution of the Ministry of labor of the Russian Federation dated 05.01.2001 No. 3 (change from 18.02.2003))
[4] SNiP 2.09.04−87	Administrative and domestic buildings
[5]	Typical branch norms of free issue of special clothes, special footwear and other individual protection means, approved by the Decree of the Ministry of labor of the Russian Federation dated 16.12.1997 G. No. 63 (amended from 17.12.2001, 26.04.2004, 16.03.2010)
[6] THE 6−09−2546−77*	Sulfur elemental. Brand high purity 16−5, 14−4 high purity, high purity 15−3
________________ * The one referred to here and hereinafter, not shown. For additional information, please refer to the link. — Note the manufacturer’s database.
[7] THE 14−8-190−91	Products high-refractory oxide — corundum, zirconium and yttrium
[8] THE 6−09−1678−95	Obestochennye filters (white, red, blue tape)
[9] THE 6−09−5295−96	Barium peroxide
[10] THE 6−09−01−255−76	Thallium nitrate
[11] THE 6−09−437−83	Cesium nitrate chemically pure, clean (cesium nitrate)
[12] THE 1769−009−44577806−2002	Tellurium ingot for thermocouples. Specifications
[13] THE 6−09−5393−88	Tin (II) chloride 2-water (tin dichloride), pure for analysis, pure

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UDC 669.24/.25:543.06:006.354 OKS 77.120.40

Key words: ore, Nickel, platinum, palladium, chemical analysis measurement tools, solution, reagent, sample, mass fraction, calibration curve, the result of the analysis, the calculation of the control