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INTERSTATE STANDARD

REAGENTS

AMMONIUM CHLORIDE

TECHNICAL CONDITIONS

Official publication

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the USSR Ministry of Chemical Industry

2. APPROVED AND ENTERED INTO EFFECT by Resolution of the State Committee of Standards of the Council of Ministers of the USSR dated April 27, 1972 No. 861

3. MS ISO 6353-2-83 (R. 5) was introduced into the standard in terms of qualification x. h.

5. REFERENCE REGULATIVE AND TECHNICAL DOCUMENTS

6. The validity period was lifted according to Protocol No. 5-94 of the Interstate Council for Standardization, Metrology and Certification (NUS 11-12-94)

7. EDITION (June 2007) with Amendments No. 1, 2, 3, approved in February 1980, July 1985, March 1990 (IUS 3-80, 10-85, 6-90)

Editor M. I. Maksimova Technical editor O. N. Vlasova Proofreader R. A. Mentova Computer layout V. I. Grishchenko

Signed for publication on June 22, 2007. Format 60x84*/8 - Offset paper. Times typeface. Offset printing. Uel. oven l. 0.93.

Academic ed. l. 0.80. Circulation 71 copies. Zach. 514.

FSUE "STANDARTINFORM", 123995 Moscow, Granatny per., 4. www.gostinfo.ru [email protected] Typed in FSUE "STANDARTINFORM" on a PC Printed in the branch of FSUE "STANDARTINFORM" - type. "Moscow Printer", 105062 Moscow, Lyalin lane, 6.

INTERSTATE STANDARD

Reagents AMMONIUM CHLORIDE Technical specifications

Reagents. Ammonium chloride. Specifications

MKS 71.040.30 OKP 26 2116 0920 01

Date of introduction 07/01/73

This standard applies to ammonium chloride.

Ammonium chloride is a white, finely crystalline powder, soluble in water.

Formula: NH 4 C1.

Molecular mass (according to international atomic masses 1971) - 53.49.

1. TECHNICAL REQUIREMENTS

1.1a. Ammonium chloride must be manufactured in accordance with the requirements of this standard according to technological regulations approved in the prescribed manner.

Official publication

1.1. In terms of physicochemical indicators, ammonium chloride must comply with the standards indicated in the table.

Reproduction is prohibited

© Standardinform, 2007

(Changed edition, Amendment No. 2, 3).

1a. SAFETY REQUIREMENTS

la. 1. Ammonium chloride can cause irritation of mucous membranes and skin.

The maximum permissible concentration in the air of the working area is 10 mg/m 3, hazard class - 3 (moderately hazardous) according to GOST 12.1.007.

1a.2. When working with the drug, it is necessary to use personal protective equipment (respirators, safety glasses, rubber gloves), and also observe personal hygiene rules.

(Introduced additionally, Amendment No. 1).

1a.Z. The premises in which work with the drug is carried out must be equipped with supply and exhaust mechanical ventilation.

The drug should be analyzed in a laboratory fume hood. In places of the greatest dust, local suction is provided.

(Changed edition, Amendment No. 3).

2. ACCEPTANCE RULES

2.2. The manufacturer determines the mass fractions of nitrates, chlorates and other oxidizing agents, arsenic and heavy metals in every 20th batch.

(Introduced additionally, Amendment No. 3).

3. METHODS OF ANALYSIS

3.1a. General instructions for conducting analysis - according to GOST 27025.

When weighing, use general purpose laboratory scales of the types VLR-200 g and VLKT-500g-M or VLE-200 g.

It is allowed to use other measuring instruments with metrological characteristics and equipment with technical characteristics no worse, as well as reagents of quality no lower than those specified in this standard.

(Changed edition, Amendment No. 3).

pipettes 4(5)-2-1(2) and 6(7)-2-25;

weighing cup SV-14/8 according to GOST 25336;

distilled water, not containing carbon dioxide; prepared according to GOST 4517; sodium hydroxide according to GOST 4328, concentration solution with (NaOH) = 0.1 mol/dm 3 (0.1 i.) and concentration solution with (NaOH) = 0.5 mol/dm 3 (0.5 i.), prepared according to GOST 25794.1; Rectified technical ethyl alcohol according to GOST 18300 of the highest grade; phenolphthalein (indicator), alcohol solution with a mass fraction of 1%, prepared according to GOST 4919.1; technical formalin according to GOST 1625, solution 1:1, previously neutralized for phenolphthalein with a solution of sodium hydroxide with a concentration of 0.1 mol/dm 3 until a pink color appears that does not disappear within 20 s, observed against the background of milk glass.

3.2.2. Carrying out analysis

About 0.8000 g of the drug is placed in a conical flask, dissolved in 40 cm 3 of water, 2-3 drops of phenolphthalein solution, 25 cm 3 of formaldehyde solution are added (pipette) and titrated from a burette with a sodium hydroxide solution of a concentration of 0.5 mol/dm 3 to pink color of the solution.

3.2.3. Processing the results

The mass fraction of ammonium chloride (X) in percent is calculated using the formula

x=Y-0.02674 100 t’

where V is the volume of sodium hydroxide solution with a concentration of exactly 0.5 mol/dm 3 used for titration, cm 3 ; t is the mass of a sample of the drug, g;

0.02674 - mass of ammonium chloride corresponding to 1 cm 3 of sodium hydroxide solution with a concentration of exactly 0.5 mol/dm 3, g.

The result of the analysis is taken as the arithmetic mean of the results of two parallel determinations, the absolute discrepancy between which does not exceed the permissible discrepancy of 0.2%.

The permissible absolute total error of the analysis results is + 0.4% with a confidence probability of P = 0.95.

3.2.2; 3.2.3. (Changed edition, Amendment No. 2, 3).

3.3. Determination of the mass fraction of water-insoluble substances

3.3.1. Reagents and glassware:

3.3.2. Carrying out analysis

50.00 g of the drug is placed in a glass and dissolved in 200 cm 3 of distilled water when heated. The glass is covered with a watch glass, heated for 1 hour in a water bath and the solution is filtered through a filter crucible, previously dried to a constant mass and weighed (the weighing result in grams is recorded to the fourth decimal place). The residue on the filter is washed with 100 cm 3 of hot water and dried in an oven at 105-110°C to constant weight.

The drug is considered to comply with the requirements of this standard if the mass of the dry residue does not exceed:

for the drug “chemically pure” - 1.0 mg; for the drug “pure for analysis” - 1.0 mg; for the “pure” drug - 5.0 mg.

Permissible relative total error of the analysis result for a drug “chemically

pure" and "pure for analysis" - +45%, for the drug "pure" - ±5% with a confidence probability of P = 0.95.

3.3.1; 3.3.2. (Changed edition, Amendment No. 3).

3.4. Determination of the mass fraction of residue after calcination

Determination of the residue after calcination is carried out according to GOST 27184. In this case, 20.00 g of the drug is placed in a platinum crucible in parts and carefully heated on an electric stove until the bulk of the drug evaporates.

The residue after calcination is stored to determine the mass fractions of calcium by and. 3.10 and magnesium according to i. 3.11.

(Changed edition, Amendment No. 1, 3).

3.5. Determination of the mass fraction of nitrates, chlorates and other oxidizing agents

In this case, 5.00 g of the drug is placed in a conical flask with a capacity of 100 cm 3 (with a 50 cm 3 mark), dissolved in 25 cm 3 of water, 1 cm 3 of hydrochloric acid solution is added, heated to a boil and boiled for 1-2 minutes. The solution is cooled and further determination is carried out using the sulfosalicylic method.

The drug is considered to comply with the requirements of this standard if the mass of iron does not exceed:

0.010 mg - for a “chemically pure” drug;

0.015 mg - for the drug “pure for analysis”;

0.050 mg - for the “pure” drug.

It is allowed to complete the definition visually.

If there is disagreement in the assessment of the mass fraction of iron, the analysis is completed photometrically. (Changed edition, Amendment No. 2).

3.10. Determination of the mass fraction of calcium (Changed edition, Amendment No. 2).

3.10.1. Equipment, reagents and solutions: flask 2-200-2 according to GOST 1770; pipettes 6(7)-2-5 and 4(5)-2-1(2); test tube P4-15-14/23 HS according to GOST 25336; distilled water according to GOST 6709;

universal indicator paper.

3.10.2. Carrying out analysis

The residue after calcination, obtained according to clause 3.4, is dissolved by heating in a water bath in 1 cm 3 of hydrochloric acid solution and 10 cm 3 of water. The solution is transferred quantitatively into a volumetric flask, the volume of the solution is adjusted to the mark with water and mixed - solution A; the solution is saved for the determination of magnesium according to paragraph 3.11.

5 cm 3 of solution A (corresponding to 0.5 g of the drug) is pipetted into a test tube, neutralized with a solution of sodium hydroxide using universal indicator paper (take-away sample), the volume of the solution is adjusted to 8 cm 3 with water, 1 cm 3 of sodium hydroxide solution is added, and mixed , add 1 cm 3 of murexide solution and mix again.

The drug is considered to comply with the requirements of this standard if the pinkish-violet color of the analyzed solution with a pink tint, observed after 1-2 minutes in transmitted light against the background of milk glass, is not more intense than the color of the reference solution prepared simultaneously with the analyzed solution and containing in the same volume: for the drug “chemically pure” - 0.005 mg Ca; for the preparation “pure for analysis” - 0.005 mg Ca; for the “pure” preparation - 0.005 mg Ca;

1 cm 3 sodium hydroxide solution and 1 cm 3 murexide solution. The color of the solution is stable for 10 minutes.

3.10.1; 3.10.2. (Changed edition, Amendment No. 2, 3).

3.11. Determination of the mass fraction of magnesium

3.11.1. Equipment, reagents and solutions:

flask Kn-1-50-14/23 THS or Kn-2-50-18 THS according to GOST 25336; pipettes 4(5)-2-1(2) and 6(7)-2-5(10); distilled water according to GOST 6709;

Type and type of container: 2-1, 2-4, 2-9, 6-1, 6-3, 11-1, 11-4.

Packing group: III, IV, V, VI, VII.

Transport containers are marked with danger signs in accordance with GOST 19433 (class 8, subclass 8.1, drawing 8, classification code 8113) and UN serial number 1759.

(Changed edition, Amendment No. 1, 2, 3).

4.2. (Deleted, Amendment No. 3).

4.3. The drug is transported by all modes of transport in accordance with the rules for the carriage of goods in force for this type of transport.

4.4. The drug is stored in closed containers in covered warehouses.

5. MANUFACTURER WARRANTY

5.1. The manufacturer guarantees that ammonium chloride meets the requirements of this standard subject to the conditions of transportation and storage.

5.2. The guaranteed shelf life of the drug is three years from the date of manufacture.