Introduction

Lead is a relatively rare element; its content is earth's crust is 1.6× 10 -3%, but lead compounds are quite often present in natural waters. The most common natural lead minerals are galena PbS, ananglesite PbSO 4, cerussite P b CO 3.

Natural sources of lead entering the aquatic environment are the dissolution processes of minerals containing lead. Anthropogenic pollution of water bodies with lead compounds is caused by their removal with wastewater from ore processing plants, mines, some metallurgical and chemical enterprises, etc. Most lead compounds (Pb) used in economic activities(NO 3 ) 2 , Pb (CH 3 COO ) 2 , PbCl 2 etc.) are relatively highly soluble, which increases the risk of contamination.

In unpolluted river and lake waters, the lead content is usually less than 10 μg/dm 3. In areas of polymetallic ore deposits, the lead content in surface waters can be increased to several tens of micrograms per cubic decimeter.

In surface waters, lead compounds are in a dissolved and suspended state. In suspension, as a rule, the sorbed form predominates. In a dissolved state, lead is found in ionic form, as well as in the form of inorganic and organic complexes.

Lead has a pronounced toxic effect on aquatic organisms and humans, disrupting metabolism and inhibiting enzymes. Lead can replace calcium in the bones when it enters the body. Organolead compounds are very toxic to living organisms. The lead content in surface waters is standardized. The maximum permissible concentration (MAC) of dissolved forms of lead in water of water bodies for household, drinking and cultural purposes is 0.01 mg/dm 3, for fishery purposes - 0.006 mg/dm 3.

GUIDANCE DOCUMENT

MASS CONCENTRATION OF LEAD IN WATER.
MEASUREMENT PROCEDURE
BY PHOTOMETRIC METHOD
WITH HEXAOXACYCLOAZOCHROME

Date of introduction - 2009-06-04

1 area of ​​use

1.1 This guidance document establishes a methodology for performing measurements (hereinafter referred to as the methodology) of the mass concentration of dissolved forms of lead in natural and treated wastewater in the range from 0.0100 to 0.0500 mg/dm 3 using the photometric method.

When analyzing water samples with a mass concentration of lead exceeding 0.0500 mg/dm 3, it is allowed to perform measurements after diluting the sample with double-distilled water so that the mass concentration of lead in the diluted sample is within the range of measured concentrations indicated above.

1.2 This guidance document is intended for use in laboratories analyzing natural and treated wastewater.

2 Normative references

This guidance document uses references to the following regulatory documents:

3 Assigned measurement error characteristics

3.1 Subject to all measurement conditions regulated by the methodology, the error characteristics of the measurement result with a probability of 0.95 should not exceed the values ​​​​given in the table.

Table 1 - Measurement range, values ​​of error characteristics and its components at the accepted probability P = 0.95

	Repeatability index (standard deviation of repeatability)	Reproducibility index (standard deviation of reproducibility)	Correctness indicator (systematic error limits)	Accuracy indicator (error limits)
	s r, mg/dm3	s R, mg/dm3	± D s, mg/dm 3	± D, mg/dm 3
From 0.0100 to 0.0500 inclusive.

When performing measurements in samples with a mass concentration of lead over 0.0500 mg/dm 3 after appropriate dilution, the measurement error limit (±D) the mass concentration of lead in the original sample is found by the formula

± D = (± D 1 ) h, (1)

where ± D 1 - indicator of the accuracy of measuring the mass concentration of lead in a diluted sample, given in the table;

h- degree of dilution.

The detection limit of lead by the photometric method with hexaoxacycloazochrome is 0.005 mg/dm 3 .

4 Measuring instruments, auxiliary devices, reagents, materials

4.1 Measuring instruments, auxiliary devices

4.1.1 Photometer or spectrophotometer of any type (KFK-3, KFK-2, SF-46, SF-56, etc.).

4.1.2 Laboratory scales high ( II ) accuracy class according to GOST 24104-2001.

4.1.3 Laboratory scales medium ( III ) accuracy class according to GOST 24104-2001 with the largest weighing limit of 200 g.

4.1.4 State standard sample of the composition of aqueous solutions of lead ions GSO 7252-96 (hereinafter referred to as GSO).

4.1.5 Measuring flasks of 2 accuracy classes according to GOST 1770-74, version 2, 2a, capacity: 25 cm 3 - 6 pcs., 100 cm 3 - 8 pcs., 500 cm 3 - 1 pc.

4.1.6 Graduated pipettes, 2 accuracy classes, versions 1, 2 according to GOST 29227-91, capacity: 1 cm 3 - 4 pcs., 2 cm 3 - 3 pcs., 5 cm 3 - 4 pcs., 10 cm 3 - 4 pcs. .

4.1.7 Pipettes with one mark 2 accuracy class 2 according to GOST 29169-91 with capacity: 5 cm 3 - 2 pcs., 10 cm 3 - 1 pc., 25 cm 3 - 1 pc., 50 cm 3 - 1 pc.

4.1.8 Dimensional cylinders 1.3 according to GOST 1770-74 with capacity: 25 cm 3 - 1 piece, 50 cm 3 - 3 pieces, 100 cm 3 - 3 pieces, 250 cm 3 - 1 piece, 500 cm 3 - 1 pc.

4.1.9 Graduated test tube version 1 (conical) according to GOST 1770-74 with a capacity of 10 cm 3 - 1 pc.

4.1.10 Glasses V-1, THS, according to GOST 25336-82, capacity: 100 cm 3 - 2 pcs., 250 cm 3 - 2 pcs., 400 cm 3 - 1 pc., 600 cm 3 - 2 pcs.

4.1.11 Conical flasks Kn, version 2, THS according to GOST 25336-82 with a capacity of 250 cm 3 - 10 pcs.

4.1.12 Weighing cups (bugs) SV-19/9, SV-24/10 according to GOST 25336-82 - 3 pcs.

4.1.21 Device for filtering samples using membrane filters.

Note- It is allowed to use other types of measuring instruments, utensils and equipment, including imported ones, with characteristics no worse than those given in.

4.2 Reagents and materials

4.2.1 Lead (II ) nitrate (lead nitrate) according to GOST 4236-77, chemical grade. (in the absence of GSO).

4.2.2 Hexaoxacycloazochrome, imported or synthesized to order.

4.2.3 Manganese (II ) nitrate, 4-water according to TU 6-09-01-613-80, analytical grade.

4.2.4 Ascorbic acid, analytical grade. according to GOST 4815-76.

4.2.5 Nitric acid according to GOST 4461-77, concentrated, chemically pure.

4.2.6 Hydrochloric acid according to GOST 3118-77, reagent grade.

4.2.7 Sulfuric acid according to GOST 4204-77, reagent grade.

4.2.8 Potassium permanganate (potassium permanganate) according to GOST 20490-75, analytical grade.

4.2.9 Potassium persulfate (potassium persulfate) according to GOST 4146-74, analytical grade.

4.2.10 Sodium hydroxide (sodium hydroxide) according to GOST 4328-77, analytical grade.

4.2.11 Sodium chloride (sodium chloride) according to GOST 4233-77, reagent grade.

4.2.12 Strong acid cation exchanger KU-2-8-chS according to GOST 20298-74 or another with equivalent characteristics.

4.2.13 Membrane filters “Vladipor MFAS-OS-2”, 0.45 microns according to TU 6-55-221-1-29-89 or another type, equivalent in characteristics.

4.2.14 Universal indicator paper according to TU 6-09-1181-76.

4.2.15 Distilled water according to GOST 6709-72.

4.2.16 Double-distilled water.

Note- It is allowed to use reagents manufactured according to other regulatory and technical documentation, including imported ones, with qualifications not lower than those specified in.

5 Measurement method

Measurements of the mass concentration of lead are based on the interaction of lead ions with hexaoxacycloazochrome (HOCAC) in a hydrochloric acid environment with the formation of colored Blue colour complex with an absorption maximum at 720 nm. Concentrating lead and separating it from accompanying components is achieved by coprecipitation with manganese dioxide.

The formula of GOTSAH is given below:

6.4 Special requirements for environmental safety not presented.

7 Operator qualification requirements

Persons with secondary vocational education, who have worked in the laboratory for at least 1 year and have mastered the technique are allowed to perform measurements and process their results.

8 Measurement conditions

When performing measurements in the laboratory, the following conditions must be met:

Ambient air temperature (22 ± 5) °C;

Atmospheric pressure from 84.0 to 106.7 kPa (from 630 to 800 mm Hg);

Air humidity no more than 80% at 25 °C;

Mains voltage (220 ± 10) V;

AC power frequency (50 ± 1) Hz.

9 Sampling and storage

Sampling for measurements of lead mass concentration is carried out in accordance with GOST 17.1.5.05 and GOST R 51592. Sampling equipment must comply with GOST 17.1.5.04 and GOST R 51592.

Samples are filtered through a 0.45 µm membrane filter, cleaned by boiling for 10 minutes in a 1% solution of nitric acid, then 10 minutes in double-distilled water. The first portions of the filtrate are discarded. The filtrate is acidified with concentrated nitric acid to pH< 2 из расчета 1 см 3 на 0,25 дм 3 воды (если этого недостаточно, добавляют еще кислоты) и хранят в полиэтиленовой (полипропиленовой) посуде не более месяца. Объем отбираемой воды не менее 0,2 дм 3 .

10 Preparing to take measurements

10.1 Preparation of solutions and reagents

10.1.1 GOCAC solution

Dissolve 0.010 g of HOCAC in 60 cm 3 of bidistilled water. Pass the solution through a column with a cation exchanger in H + - form and collect it in a volumetric flask with a capacity of 100 cm 3. The column is washed with bidistilled water, collecting the wash water in the same volumetric flask, adjust the volume of the solution to the mark and mix. The GOTSAH solution is stored in the refrigerator for no more than 10 days.

10.1.2 Nitric acid solution, 1 mol/dm 3

Add 36 cm 3 of concentrated nitric acid to 465 cm 3 of bidistilled water and mix. The solution is stable.

10.1.3 Nitric acid solution, 1%

Mix 5.5 cm 3 of concentrated nitric acid with 500 cm 3 of bidistilled water. The solution is stable. Used to clean filters.

10.1.4 Hydrochloric acid solution, 4 mol/dm 3

Mix 85 cm 3 of concentrated hydrochloric acid with 165 cm 3 of distilled water.

10.1.5 Hydrochloric acid solution, 1 mol/dm 3

Mix 21 cm 3 of concentrated hydrochloric acid with 230 cm 3 of distilled water.

10.1.6 Hydrochloric acid solution, 0.1 mol/dm 3

Dissolve 4.3 cm 3 of concentrated hydrochloric acid in 500 cm 3 of bidistilled water.

10.1.7 Manganese nitrate solution, 10%

Dissolve 14 g of Mn (NO 3 ) 2 × 4H2O in 86 cm 3 of bidistilled water. Store in a bottle with a ground-in stopper for no more than 1 month.

10.1.8 Potassium permanganate solution, 1%

Dissolve 1.0 g KMnAbout 4 in 100 cm 3 of bidistilled water. Store in a dark glass bottle with a ground stopper for no more than 7 days.

10.1.9 Potassium persulfate solution, 5%

47 cm 3 of bidistilled water, 0.5 cm 3 of concentrated sulfuric acid, 2.5 g of potassium persulfate are placed in a conical flask with a capacity of 250 cm 3 and stirred until dissolved. The solution is stored in a bottle with a ground-in stopper for no more than 10 days.

10.1.10 Solution ascorbic acid, 10%

Dissolve 10 g of ascorbic acid in 90 cm 3 of bidistilled water and add 1 cm 3 of a 1 mol/dm 3 solution of nitric acid. Store in a dark bottle in the refrigerator for no more than 5 days.

10.1.11 Sodium hydroxide solution, 1 mol/dm 3

Dissolve 20 g of sodium hydroxide in 500 cm 3 of distilled water. Store in plastic containers.

10.1.12 Preparing a column with cation exchange resin H+-form

Preparation and regeneration of a column with cation exchanger in H + - form are given in the Appendix.

The column is used to pass the HOCAC solution 10 - 12 times and then regenerated.

10.2 Preparation of calibration solutions

10.2.1 Calibration solutions are prepared from GSO with a mass concentration of lead of 1.00 mg/cm 3 . The GSO ampoule is opened and its contents are transferred to a dry, clean, graduated test tube. To prepare a calibration solution with a mass concentration of lead of 0.0500 mg/cm 3, take 5.0 cm 3 of the sample using a clean, dry pipette with one mark with a capacity of 5 cm 3 and transfer it to a volumetric flask with a capacity of 100 cm 3. Add 0.4 cm 3 of concentrated nitric acid, adjust the volume in the flask to the mark with bidistilled water and mix. The solution is stored in a tightly closed bottle in the refrigerator for no more than 6 months.

10.2.2 To prepare a calibration solution with a mass concentration of lead of 0.0010 mg/cm 3, use a graduated pipette with a capacity of 2 cm 3 to take 2.0 cm 3 of the calibration solution with a mass concentration of lead of 0.0500 mg/cm 3, place it in a volumetric flask with a capacity 100 cm 3, bring to the mark with bidistilled water and mix. The solution is stored for no more than three days.

10.2.3 If the mass concentration of manganese in the GSO is not exactly 1.00 mg/cm 3, calculate the mass concentration of lead in the resulting calibration solutions in accordance with the concentration of a specific sample.

10.2.3 In the absence of GSO, it is allowed to use a certified lead solution prepared from lead nitrate. The method for preparing the certified solution is given in the Appendix.

10.3 Establishment of calibration dependence

10.3.1 To prepare calibration samples, 0; 0; 1.0; 2.0; 3.0; 4.0; and 5.0 cm 3 of lead calibration solution with a mass concentration of 0.0010 mg/cm 3 and bring the volume of the solution to the mark with bidistilled water. The mass concentration of lead in the resulting solutions will be 0; 0.010; 0.020; 0.030; 0.040; 0.050 mg/dm3.

10.3.2 Solutions from volumetric flasks are quantitatively transferred into conical flasks with a capacity of 250 cm 3, rinsing the volumetric flasks with 2 cm 3 of bidistilled water, then add 0.3 cm 3 of concentrated nitric acid, 1 cm 3 of potassium persulfate solution to each flask and thoroughly stir. The contents of each flask are transferred in approximately equal parts into two or more quartz tubes (depending on the capacity of the tubes), the tubes are placed in a device for treating water samples with UV irradiation and irradiated for 20 minutes.

After irradiation, the solutions are quantitatively transferred into conical flasks with a capacity of 250 cm 3 and then they are processed and the optical density is measured as described in -.

10.3.3 The calibration dependence of the optical density of samples on the mass concentration of lead is calculated by the least squares method or using a computer program.

The calibration dependence is established when using a new batch of GODAH or other measuring instrument, but at least once a year.

10.4 Monitoring the stability of the calibration characteristic

10.4.1 The stability of the calibration characteristic is monitored when preparing a new solution of GOCAC. Control means are samples used to establish a calibration relationship (at least three). The calibration characteristic is considered stable if the condition is met

If the stability condition is not met for one calibration sample, it is necessary to re-measure this sample to eliminate the result containing a gross error. If the condition is not met again, the causes of instability are determined, eliminated, and the measurement is repeated using other samples provided for in the method. If the calibration characteristic again does not satisfy condition (), a new calibration dependence is established.

10.4.2 When condition () is met, the sign of the difference between the measured and assigned values ​​of the mass concentration of lead in the samples is taken into account. This difference must have both positive and negative values, but if all values ​​have the same sign, this indicates the presence of a systematic deviation. In this case, it is necessary to establish a new calibration relationship.

11 Taking measurements

11.1 Using a measuring cylinder with a capacity of 100 cm 3, take 100 cm 3 of filtered test water, place it in a conical flask with a capacity of 250 cm 3, add 0.3 cm 3 of concentrated nitric acid (if the sample was preserved, do not add nitric acid) and 1 cm 3 potassium persulfate solution.

The resulting mixture is transferred in approximately equal parts into two or more quartz tubes (depending on the capacity of the latter), placed in a device for treating water samples with UV irradiation and irradiated for 20 minutes.

If the optical density of the sample is higher than that for the last point of the calibration curve, repeat the measurement by taking a smaller aliquot of the analyzed water and diluting it to 100 cm 3 with bidistilled water. An aliquot of the water sample for dilution is selected so that the lead concentration in the diluted sample is in the range from 0.030 to 0.050 mg/dm 3 .

11.4 The interfering influence of suspended and colloidal substances is eliminated by preliminary filtering of the sample. Possible interfering influences of the sample matrix are eliminated by destroying organic substances by UV irradiation and separating lead from water by coprecipitation with manganese dioxide in the form PbO2.

12 Calculation of measurement results

12.1 Mass concentration of lead X , mg/dm3, in the analyzed water sample is calculated using the formula

(3)

where C is the mass concentration of lead, found from the calibration curve, mg/dm 3 ;

V - volume of a water sample aliquot taken for analysis, cm3.

12.2 The measurement result in documents providing for its use is presented in the form

X ± D, mg/dm 3 (P = 0.95), (4)

where ± D- limits of the error characteristic of the measurement result for a given mass concentration of lead, mg/dm 3 (see table).

The numerical values ​​of the measurement result must end with a digit of the same digit as the values ​​of the error characteristic; the latter should not contain more than two significant figures.

12.3 It is acceptable to present the result in the form

X ± D l (P = 0.95) providedD l< D, (5)

where ± D l - limits of the error characteristics of the measurement results, established during the implementation of the methodology in the laboratory and ensured by monitoring the stability of the measurement results, mg/dm 3.

Note- It is permissible to establish the characteristic error of measurement results when introducing a technique in a laboratory based on the expression D l = 0.84 D with subsequent clarification as information accumulates in the process of monitoring the stability of measurement results.

12.4 The measurement results are documented in a protocol or journal entry, according to the forms given in the Laboratory Quality Manual.

13 Quality control of measurement results when implementing the technique in the laboratory

13.1 General provisions

13.1.1 Quality control of measurement results when implementing the methodology in the laboratory includes:

Monitoring the stability of measurement results (based on monitoring the stability of the error).

13.1.2 The frequency of operational monitoring by the performer of the measurement procedure, as well as the implemented procedures for monitoring the stability of the results of measurements performed, are regulated in the Laboratory Quality Manual

13.2 Algorithm for operational control of the measurement procedure using the additive method

13.2.1 Operational control by the performer of the measurement procedure is carried out by comparing the results of a separate control procedure K to with the control standard K.

13.2.2 The result of the control procedure K k, mg/dm 3, is calculated using the formula

(6)

where X ¢ - the result of a control measurement of the mass concentration of lead in a sample with a known additive, mg/dm 3 ;

X is the result of measuring the mass concentration of lead in the working sample, mg/dm 3 ;

C is the amount of the additive, mg/dm3.

13.2.3 Control standard K, mg/dm3, is calculated using the formula

(7)

Where D lx ¢ - values ​​of the error characteristics of the measurement results established in the laboratory when implementing the method, corresponding to the mass concentration of lead in the sample with the additive, mg/dm 3 ;

D lx - values ​​of the error characteristics of the measurement results established in the laboratory during the implementation of the method, corresponding to the mass concentration of lead in the working sample, mg/dm 3.

Note- It is permissible to calculate the control standard to use the values ​​of the error characteristics obtained by calculation using the formulas D lx ¢ = 0,84D X ¢ , And D lx = 0.84 D X.

13.2.4 If the result of the control procedure satisfies the condition

14.2 If the reproducibility limit is exceeded, methods for assessing the acceptability of measurement results can be used in accordance with section 5 of GOST R ISO 5725-6 or MI 2881.

14.3 Acceptability testing is carried out when it is necessary to compare measurement results obtained by two laboratories.

Appendix A

(required)

Preparation and regeneration of a cation exchanger column

Soak 25 - 30 g of dry cation exchange resin for 1 - 2 days. in a saturated solution of sodium chloride in distilled water (70 g of sodium chloride is dissolved in 200 cm 3 of water). Then the sodium chloride solution is drained, the cation exchanger is washed 2-3 times with distilled water and the cation exchanger is filled with a solution of hydrochloric acid 4 mol/dm 3 for a day. The colored solution of hydrochloric acid is drained, the cation exchanger is washed 2-3 times with distilled water by decantation, and the treatment of the cation exchanger with a solution of hydrochloric acid is repeated again until the solution above the cation exchanger ceases to be colored. yellow. After this, the cation exchanger is transferred to the column along with water so that no air bubbles form. The height of the cation exchanger layer in the column should be about 15 cm. First, a little distilled water is poured into the column. Excess water when filling the column is periodically drained through the tap. After filling, 30 cm 3 of a 1 mol/dm 3 sodium hydroxide solution, distilled water and a 1 mol/dm 3 hydrochloric acid solution are passed through the column with the cation exchanger at a rate of 1 - 2 drops per second, repeating the procedure 8 - 10 times. The cation exchanger treatment is completed by passing 30 cm 3 of hydrochloric acid solution. After this, wash the column with bidistilled water to pH 5 on universal indicator paper, passing water at the maximum possible speed. When not in use, the column is kept hermetically sealed. The cation exchanger must be constantly under a layer of water.

Periodically, the column is regenerated by passing 50 cm 3 of a 1 mol/dm 3 hydrochloric acid solution and washing with bidistilled water.

Cation exchange resin (both dry and wet) ages over time and loses its ion-exchange properties. To check the suitability of the cation exchanger, prepare a solution of sodium chloride with a molar concentration of 0.010 mol/dm 3, for which 0.0585 g of sodium chloride is weighed and dissolved in distilled water in a volumetric flask with a capacity of 100 cm 3. After initial preparation or after regeneration, 50 cm 3 of distilled water is passed through the column at a rate of 1 - 2 drops per second. The first 20 - 25 cm 3 of water passing through the column is discarded, the next portion of about 25 cm 3 is collected in a glass with a capacity of 50 cm 3 and the pH of the cationized water is measured. After this, the prepared sodium chloride solution is passed at the same speed, the first 20 - 25 cm 3 of the solution that passes through the column is discarded, and the next portion is collected in a glass and the pH is also measured. Due to the replacement of sodium ions in the solution when passing through a cation exchanger with hydrogen ions, the pH of the solution decreases compared to cationized distilled water. If the quality of the cation exchanger is satisfactory, the difference in pH value should be 2.5 - 3 units.

Methodology for preparing a certified lead solution AP1-R b to establish the calibration characteristics of instruments and control the accuracy of measurements of the mass concentration of lead using the photometric method

B.1 Purpose and scope

This methodology regulates the procedure for preparing a certified lead solution intended to establish the calibration characteristics of instruments and control the accuracy of the results of measurements of the mass concentration of lead in natural and treated wastewater using the photometric method.

B.2 Metrological characteristics

B.2.1 Certified value of the mass concentration of lead in the AP1-P solution b is 1,000 mg/cm 3 .

B.2.2 Error limits for establishing the certified value of the mass concentration of lead in the AP1-P solution capacity: 25 cm 3 - 1 pc.

Weigh in a bottle on a high-precision laboratory scale 0.799 g Pb(NO3 ) 2 accurate to the fourth decimal place, transfer it quantitatively into a volumetric flask with a capacity of 500 cm 3, dissolve it in a small amount of double-distilled water, add 2 cm 3 of concentrated nitric acid, adjust the volume of the solution to the mark with double-distilled water and mix.

B.6 Calculation of metrological characteristics of a certified solution AP 1-Pb

B.6.1 The certified value of the mass concentration of lead C, mg/cm 3, in solution is calculated using the formula

(B.1)

where m - mass of lead nitrate sample, g;

207.2 - molar mass of lead, g/mol;

331.2 - molar mass of lead nitrate Pb (NO 3 ) 2 , g/mol.

B.6.2 Calculation of the error in preparing a certified solutionD, mg/cm 3, perform according to the formula

(B.2)

Where m- mass fraction of the main substance Pb(NO 3 ) 2 assigned to a reagent grade reagent, %;

D m - limit value possible deviation mass fraction of the main substance in the reagent from the assigned valuem, %;

D m - maximum possible weighing error, g;

m - mass of lead nitrate sample, g;

V - volumetric flask capacity, cm 3;

D V - the limit value of the possible deviation of the capacity of the volumetric flask from the nominal value, cm 3.

The limits of possible error values ​​for the preparation of a certified solution are equal to

B.7 Safety requirements

Must be observed General requirements safety precautions when working in chemical laboratories.

B.8 Operator qualification requirements

A certified solution can be prepared by an engineer or laboratory technician with secondary vocational education, who has undergone special training and has worked in a chemical laboratory for at least a year.

B.9 Labeling requirements

The bottle with the certified solution must be affixed with a label indicating the symbol of the solution, the mass concentration of lead, the error in its determination and the date of preparation.

B.10 Storage conditions

Certified solution AP1-PbStore in a tightly closed bottle for no more than 6 months.

Federal Service for Hydrometeorology
and monitoring environment

GOVERNMENT INSTITUTION

HYDROCHEMICAL INSTITUTE

CERTIFICATE

on certification of measurement techniques № 102.24-2008

Methodology for measuring the mass concentration of lead in waters using the photometric method with hexaoxacycloazochrome,

developed by the State Institution Hydrochemical Institute

and regulated by RD 52.24.448-2009. Mass concentration of lead in waters. Methodology for performing measurements using the photometric method with hexaoxacycloazochrome

certified in accordance with GOST R 8.563-96.

Certification was carried out based on the results of experimental studies.

As a result of the certification, it was established that the measurement technique complies with the metrological requirements imposed on it and has the metrological characteristics given in tables and.

Table 1 - Measurement range, values ​​of measurement error characteristics and its components at the accepted probability P = 0.95

Table 2 - Measurement range, values ​​of repeatability and reproducibility limits at the accepted probability P = 0.95

When implementing the technique in the laboratory, the following is provided:

Operational control by the performer of the measurement procedure (based on the assessment of the error when implementing a separate control procedure);

Monitoring the stability of measurement results (based on monitoring the stability of repeatability, intra-laboratory precision, error).

The algorithm for operational control by the performer of the measurement procedure is given in RD 52.24.448-2009.

The frequency of operational monitoring and procedures for monitoring the stability of measurement results are regulated in the Laboratory Quality Manual.

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1 PHOTOMETRIC DETERMINATION OF LEAD IN AQUEOUS SOLUTIONS BY REACTION WITH XYLENOL ORANGE N.V. Kuleshova, L.A. Savina Nizhny Novgorod State University them. N.I. Lobachevsky A method has been developed for the photometric determination of lead (II) in aqueous solutions by reaction with xylenol orange. Preliminary conversion of lead (II) into acetate form increases the sensitivity of determination and reduces the detection limit. To increase selectivity, sorption separation of lead (II) on the Wofatit cation exchanger was proposed. The detection limit using our method is 0.2 μg/15 ml sample. INTRODUCTION In terms of the scale of emissions into the atmosphere, lead ranks first among microelements. The development of scientific and methodological aspects of monitoring the content of this metal, toxic in all its water-, acid- and alkali-soluble forms, is one of the urgent tasks in the field of environmental protection. The volume of scientific information on this issue is significant and continues to grow. Currently, to determine heavy metals in environmental objects, the entire existing arsenal of physical, chemical and physicochemical methods of analysis is used, the results of which are important for the development and coordination of environmental protection measures. The use of a particular method is determined by the lead content in the analyzed object, as well as the required accuracy, determination time and technical equipment of the laboratory. The photometric method of analysis combines reliability and versatility with simplicity and accessibility. The purpose of this work was to select a suitable reagent for the photometric determination of microgram quantities of lead (II) and to optimize the working conditions with it when analyzing various objects. EXPERIMENTAL The work used lead nitrate Pb(NO 3) 2, ammonium acetate CH 3 COONH 4, methenamine, copper sulfate Cu(SO 4) 5H 2 O, zinc nitrate Zn(NO 3) 2 reagent grade. and ch.d.a. Dyes: xylenol orange (0.05% aqueous solution), glycinthymol blue (0.03% aqueous solution), sulfarsazen (0.05% solution in 0.05 M Na 2 B 4 O 7) and STEAM (0.05% alcohol solution). Solutions of hydrochloric, sulfuric, acetic acids and an aqueous solution of ammonia were prepared from concentrated ones by diluting with distilled water. Initial solutions of salts were prepared by precise weighing; solutions of lower concentrations were prepared by serial dilution of the original ones. Dye solutions are stable for 3–4 days. Lead acetate solutions were prepared immediately before use. 219

2 Photometric measurements were carried out using a KFK-3 photocolorimeter; the acidity of solutions was controlled using a pH-150 potentiometer. DISCUSSION OF RESULTS To fully characterize a colored complex compound used in photometric analysis, it is necessary to know the conditions for the formation of the complex (pH, concentration of the reagent and its amount, time to reach reaction equilibrium, etc.), its composition, molar light absorption coefficient, region of subjection to Bouguer’s law Lambert Behr. The study of dyes began with studying the absorption spectra of solutions of dyes and the products of their interaction with lead solutions at different pH values ​​(Fig. 1). Lead (II) in aqueous salt solutions tends to form anionic complex ions. The strength of acetate is characterized by the values ​​pk 3 = 2.4; and pk 4 = 2.1. Wavelength, nm Fig. 1. Absorption spectra of xylenol orange and its complexes with lead in various solutions (L = 2 cm): a acetate solution; b dye solution; into an aqueous solution. It has been established that xylenol orange forms colored compounds not only with Pb 2+, but also with acetate complex lead ions. The composition of these products was determined using the isomolar series method. Lead (2+) forms a 1:1 complex with the reagent, and lead in acetate form forms a 1:2 complex. Their stability has been assessed. Time to reach equilibrium is 20 minutes. The influence of various factors on the sensitivity coefficient for the determination of lead with xylenol orange was studied. The composition of buffer solutions that maintain the optimal pH value = 5.6 has a significant impact on the type of calibration dependencies (Fig. 2). Preliminary conversion of lead into acetate form and the use of ammonium acetate buffer increases the sensitivity coefficient by 2 times (the molar light extinction coefficient increases from to l/mol cm). In addition, the linear section of the calibration graph expands into the region of lower concentrations. Under these conditions, the selectivity of photomet-220 increases

3 ric determination of lead, because most metals do not form complex ions with acetate (Table 1). It has been established that over time the calibration characteristic shifts to the region of lower optical densities parallel to the original straight line. To obtain reproducible results, it should be taken into account that the 1:2 chelate is less stable than 1:1. Therefore, measurements must be carried out within a certain period of time after equilibrium is achieved. The determination of lead in aqueous solutions was carried out graphically (according to a previously constructed calibration graph) or analytically (according to the equation of the calibration dependence (Fig. 3). For this purpose, a series of 10 6 g Pb/15 ml was prepared. Fig. 2. Effect of the composition of the buffer solution on the type calibration dependencies: a Pb (II) acetate, CH 3 COOH + NH 4 OH; b Pb (II), CH 3 COOH + NH 4 OH; c Pb (II) acetate. lemon acid+NaOH; g Pb(II), citric acid + NaOH Comparative characteristics dyes for the photometric determination of lead (II) Linear region, Table 1 Sensitivity, pH t Composition Dye PrO λ Equation GG (lead solution) µg Pb/15 g/15 ml equal, min. eff., complex nm l/(mol cm) ml Sulfarsazen y = 8800x ± , :1 (acetate) +0.23 PAR y = 25600x ±820 0.5 7 1, :1 (aqueous) + 0.25 GTS ( acetate) (aqueous) Xylenol orange (acetate) (aqueous) y = 36000x+ + 0.26 y = 25000x+ + 0.20 y = 49800x+ +0.18 y = 13500x+ +0, ± ± ±500 0.8 7, 8 5.6 5, :2 1:2 1:2 1:1 221

4 dilution solutions from a standard lead solution (1 μg/ml), prepared by diluting the original solution of ammonium acetate (1 mol/l). For this purpose, from 0.5 to 7 ml of a standard solution were taken, 1 ml of a 0.05% solution of xylenol orange, 3 ml of an acetate-ammonia buffer mixture (pH 5.6) were added, and the volume was adjusted to 15 ml with distilled water. Optical density measurements were carried out after minutes. To determine the lead content in the test solution, 1–3 ml of it was treated in the same way as calibration solutions, adding 5 ml of 1 M ammonium acetate to the sample. m 10 6 g Pb/15 ml Fig. 3. Calibration dependence for the determination of Pb (II): a) solution of Pb (II) acetate; b) aqueous solution of Pb (II) The accuracy of lead determination using the developed method was confirmed by ionometry with Pb-SE (Table 2). 222 Table 2 Assessment of the accuracy of the determination of lead in aqueous solutions (n ​​= 4, p = 0.95) Entered, Determined, μg μg ionometrically S r photometrically S r 1.00 1.03 ± 0.04 0.09 0.99 ± 0.25 0.06 4.00 4.06 ± 0.05 0.08 4.02 ± 0.02 0.03 7.00 6.96 ± 0.04 0.06 7.01 ± 0.03 0 .05 10.00 9.81 ± 0.92 0.09 10.20 ± 0.20 0.03 25.00 25.70 ± 1.50 0.06 24.98 ± 0.50 0.02 With photometric In determining lead by reaction with xylenol orange, the main interfering ions are Zn 2+ and Cu 2+. To eliminate the interfering influence of these ions, the processes of sorption and desorption of lead on some organic cation exchangers have been studied. Before starting work, the sorbents were placed in a beaker, treated for 20 minutes with a solution of HCl (1:1), washed with water until the wash water was neutral and filled with 1 M CH 3 COONH 4. After 30 minutes of stirring on a magnetic stirrer, the sorbent was again washed with water and dried with a filter. paper and added a precisely measured volume of an aqueous solution of lead nitrate of known concentration (pH 5) into a glass. The contents of the glass were stirred with a magnetic stirrer for an hour, then the solution was drained and a sample was taken to determine the residual lead content

5 after sorption. The sorbent was washed with a portion of water, dried with filter paper and filled with a 1 M solution of ammonium acetate heated to 60 C. The mixture was kept in a water bath (60 C) for 30 minutes, stirring occasionally. After the specified time, a sample was taken again to determine the lead content and assess the degree of desorption. The results are presented in table. 3. To isolate lead from mixed solutions, Wofatit was selected, for which sorption and desorption are maximum. Table 3 Degree of sorption and desorption of lead on ion exchange resins, % Process IRA Dowex KU-1 KU-2 KRS-10T KRS-2P Wofatit Desorption Sorption The possibility of separating lead from zinc and copper ions that interfere with photometric determination was assessed on the selected sorbent. The maximum molar ratios of ions, the interfering influence of which is eliminated by separation of lead on the Wofatit sorbent, are given in Table. 4. Table 4 Limit molar ratios of ions that do not interfere with the determination of lead Ions Zn 2+ Cu 2+ Zn 2+ + Cu 2+ C(Pb 2+)/C(Me 2+) 1:12 1:15 1:13 Developed The method for determining lead by reaction with xylenol orange was used to study the sorption capabilities of the preparations “Ukrop” and “Petrushka” from the Biofit company. For this purpose, 2 g of the drug was poured into 20 ml of distilled water and a 0.5 M solution of hydrochloric acid was added to pH 3.5 (acidity level of gastric juice). Then a sample of lead nitrate was added to the system and the sample was stirred on a magnetic stirrer. After 3 hours, the solution was filtered and 0.5–1.0 ml was taken to determine the lead in it. The mass fraction (%) of lead sorbed on a plant preparation was calculated using the formula: W = (m i /m j) 100, where m i is the mass of lead in the solution after sorption; m j is the mass of lead (2+) introduced into the solution. The results of the determination are presented in table. 5. Grows. drug Parsley Dill Table 5 Sorption of lead herbal preparations company "Biofit" Injected salt Mass fraction of sorbed Pb 2+, % Pb(NO 3) 2 Pb 2+ in a separate average value experience 0.0244 0.97 0.0309 0.52 93.25 0.0315 0.2 0.031 0.66 89.43 223

6 The results obtained led to the conclusion that these drugs, in addition to their main properties as dietary supplements, also exhibit detoxifying properties. REFERENCES 1. Maistrenko V.N., Khamitov R.Z., Budnikov G.K. Ecological and analytical monitoring of supertoxicants. M.: Chemistry, p. 2. Analytical complex for the determination of lead in environmental and biological objects / S.M. Lyapunov, I.F. Seregina, etc. // Problems of the environment and natural resources: Review inform / VINITI S Lukin A.M., Petrova G.S. // Journal. analyte chemistry T. S. Gurkina T.V., Igoshkin A.M. // Journal. analyte chemistry T S Shvoeva O.P., Dedkova V.T., Savvina S.B. // Journal. analyte chemistry T S Akhmedli M.I., Ayubaeva M.A., Azimova R.S. // Azerbaijan Chem. journal S Skachkova N.V., Kuleshova N.V. Manufacturing and research of liquid ion-selective electrodes for the determination of lead // V conference of young chemical scientists Nizhny Novgorod: Abstract. report N. Novgorod, S

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Essay

The course work contains: ___ pages, 4 tables, 2 figures, 8 literary sources. The object of research in the course work is complex food products chemical composition.

The purpose of the work is to determine the lead content in food products and compare it with the MPC.

The research method is atomic absorption.

Sample preparation methods are given. Data on the content of lead compounds in food objects (objects) were analyzed and summarized.

Area of ​​application: analytical and toxicological chemistry, laboratories for standardization and quality of food products produced by light industry, pharmaceutical chemistry.

Keywords: LEAD, ATOMIC ABSORPTION SPECTROSCOPY, ABSORPTION, STANDARD SOLUTION, CALIBRATION GRAPH, CONTENTS, MPC

Introduction

1. Literature review

1.3 Sample preparation

2. Experimental part

conclusions

Introduction

The use of materials containing lead and its compounds has led to the pollution of many environmental objects. Determination of lead in metallurgical products, biological materials, soils, etc. presents difficulties because it is usually accompanied by other divalent metals. To solve such an analytical problem, the atomic absorption method of determination has become widespread due to the availability of equipment, high sensitivity and sufficient accuracy.

Food products may contain not only useful material, but also quite harmful and dangerous for the human body. Therefore, the main task of analytical chemistry is food quality control.

Namely, this course work uses the atomic absorption method for determining lead in coffee.

1. Literature review

1.1 Chemical properties lead

In the periodic table D.I. Mendeleev lead is located in group IV, main subgroup and has an atomic weight of 207.19. Lead in its compounds can be in the +4 oxidation state, but the most characteristic for it is +2.

In nature, lead occurs in the form of various compounds, the most important of which is the lead luster PbS. The abundance of lead in the earth's crust is 0.0016 wt. %.

Lead is a bluish-white heavy metal with a density of 11.344 g/cm 3. It is very soft and can be easily cut with a knife. Lead melting point 327.3 O C. In air, lead quickly becomes covered with a thin layer of oxide, protecting it from further oxidation. In the voltage series, lead comes immediately before hydrogen; its normal potential is - 0.126 V.

Water by itself does not react with lead, but in the presence of air, lead is gradually destroyed by water to form lead hydroxide:

Pb+O 2+ H2 O=2Pb(OH) 2

However, when it comes into contact with hard water, lead becomes covered with a protective film of insoluble salts (mainly lead sulfate and basic lead carbonate), which prevents further action of water and the formation of hydroxide.

Dilute hydrochloric and sulfuric acids do not act on lead due to the low solubility of the corresponding lead salts. Lead easily dissolves in nitric acid. Organic acids, especially acetic acid, also dissolve lead in the presence of atmospheric oxygen.

Lead also dissolves in alkalis, forming plumbites.

1.2 Physiological role of lead

The metabolism of lead in humans and animals has been studied very little. Biological role it is also not completely clear. It is known that lead enters the body with food (0.22 mg), water (0.1 mg) and dust (0.08 mg). Typically, the lead content in a man's body is about 30 µg%, and in women it is about 25.5 µg%.

From a physiological point of view, lead and almost all its compounds are toxic to humans and animals. Lead, even in very small doses, accumulates in the human body, and its toxic effect gradually increases. When lead poisoning occurs, gray spots appear on the gums and functions are impaired. nervous system, there is pain in internal organs. Acute poisoning leads to severe damage to the esophagus. For people who work with lead, its alloys or compounds (for example, printing workers), lead poisoning is an occupational disease. The dangerous dose for an adult lies in the range of 30-60 g Pb (CH3COO) 2 * 3H 2ABOUT .

1.3 Sample preparation

The selection and preparation of laboratory samples is carried out in accordance with the normative and technical documentation for this type of product. Two parallel samples are taken from the combined laboratory sample.

Products with a high sugar content (confectionery, jams, compotes) are treated with sulfuric acid (1: 9) at the rate of 5 cm 3 acid per 1 g of dry matter and incubated for 2 days.

Products with a fat content of 20-60% (cheese, oil seeds) are treated with nitric acid (1:

) based on 1.5 cm 3 acid per 10 g of dry matter and incubated for 15 minutes.

Samples are dried in an oven at 150 O C (if there are no aggressive acid fumes) on an electric stove with low heat. To speed up sample drying, simultaneous irradiation of samples with an IR lamp can be used.

Dried samples are carefully charred on an electric stove or gas burner until the emission of smoke stops, preventing ignition and emissions.

Place the crucibles in a cold electric furnace and increase its temperature by 50 O Every half hour, bring the oven temperature to 450 O C. At this temperature, mineralization is continued until gray ash is obtained.

The ash cooled to room temperature is moistened dropwise with nitric acid (1:

) based on 0.5-1 cm 3 weighed acids, evaporated in a water bath and dried on an electric stove with low heat. Place the ash in an electric furnace and bring its temperature to 300 O C and kept for 0.5 hours. This cycle (acid treatment, drying, ashing) can be repeated several times.

Mineralization is considered complete when the ash becomes white or slightly colored without charred particles.

Wet mineralization. The method is based on the complete decomposition of organic substances of the sample when heated in a mixture of concentrated nitric acid, sulfuric acid and hydrogen peroxide and is intended for all types of food products butter and animal fats.

A weighed portion of liquid and puree products is added to a flat-bottomed flask, wetting the walls of a 10-15 cm glass 3bidistilled water. You can take the sample directly into a flat-bottomed flask.

A sample of solid and pasty products is taken onto an ash-free filter, wrapped in it and placed with a glass rod on the bottom of a flat-bottomed flask.

Drink samples are taken with a pipette, transferred to a Kjeldahl flask and evaporated on an electric stove to 10-15 cm3 .

A weighed portion of dry products (gelatin, egg powder) is placed in a flask and 15 cm is added 3bidistilled water, stir. Gelatin is left for 1 hour to swell.

Sample mineralizationMineralization of samples of raw materials and food products except vegetable oils, margarine, edible fats:

Nitric acid is added to the flask to calculate 10 cm 3for every 5 g of product and incubate for at least 15 minutes, then add 2-3 clean glass beads, close with a pear-shaped stopper and heat on an electric stove, first weakly, then more strongly, evaporating the contents of the flask to a volume of 5 cm3 .

Cool the flask, add 10 cm 3nitric acid, evaporate to 5 cm 3. This cycle is repeated 2-4 times until the brown fumes stop.

Add 10 cm to the flask 3nitric acid, 2 cm 3sulfuric acid and 2 cm 3hydrogen peroxide for every 5 g of product (mineralization of dairy products is carried out without adding sulfuric acid).

To remove residual acids, add 10 cm 3double-distilled water, heat until white vapor appears and then boil for another 10 minutes. Cool. Adding water and heating is repeated 2 more times.

If a precipitate forms, add 10 cm 3bidistilled water, 2 cm 3sulfuric acid, 5 cm 3hydrochloric acid and boil until the precipitate dissolves, adding evaporating water. After dissolving the precipitate, the solution is evaporated in a water bath to wet salts.

Mineralization of vegetable oils, margarine, edible fats:

lead food chemistry

The flask with the sample is heated on an electric stove for 7-8 hours until a viscous mass is formed, cooled, and 25 cm 3nitric acid and carefully heat again, avoiding violent foaming. After foaming stops, add 25 cm 3nitric acid and 12 cm 3hydrogen peroxide and heat until a colorless liquid is obtained. If the liquid darkens, periodically add 5 cm 3nitric acid, continuing heating until mineralization is complete. Mineralization is considered complete if the solution remains colorless after cooling.

Acid extraction. The method is based on the extraction of toxic elements with dilute (1:

) by volume with hydrochloric acid or diluted (1: 2) by volume with nitric acid and is intended for vegetable and butter oils, margarine, edible fats and cheeses.

Extraction is carried out in a heat-resistant sample of the product. A 40 cm cylinder is added to the flask 3solution of hydrochloric acid in double-distilled water (1:

) by volume and the same amount of nitric acid (1: 2). Several glass beads are added to the flask, a refrigerator is inserted into it, placed on an electric stove, and boiled for 1.5 hours from the moment of boiling. Then the contents of the flask are slowly cooled to room temperature without removing the refrigerator.

The flask with the extraction mixture of butter, fats or margarine with acid is placed in a cold water bath to solidify the fat. The hardened fat is pierced with a glass rod, the liquid is filtered through a filter moistened with the acid used for extraction into a quartz or porcelain bowl. The fat remaining in the flask is melted in a water bath, add 10 cm 3acids, shake, cool, after cooling the fat is calcined and the liquid is poured through the same filter into the same bowl, then washed 5-7 cm 3bidistilled water.

Extraction mixture vegetable oil with acid, transfer to a separatory funnel. The flask is rinsed 10 cm 3acid, which is poured into the same funnel. After phase separation, the lower aqueous layer is poured through an acid-soaked filter into a quartz or porcelain bowl, the filter is washed 5-7 cm 3bidistilled water.

The extraction mixture of cheese and acid is filtered through an acid-soaked filter into a quartz or porcelain bowl. The flask is rinsed 10 cm 3acid, which is filtered through the same filter, then the filter is washed 5-7 cm 3bidistilled water.

The filtered extract is carefully evaporated and charred on an electric stove, and then ashed in an electric oven.

1.4 Lead determination methods

1.4.1 Concentration of trace amounts of lead ion using nanometer particles of titanium dioxide (anatase) for the purpose of their subsequent determination by inductively coupled plasma atomic emission spectrometry with electrothermal evaporation of the sample

Inductively coupled plasma atomic emission spectrometry ( ISP-AES) -a widely used and very promising method of elemental analysis. However, it has some disadvantages, including relatively low detection sensitivity, low sputtering efficiency, spectral interference and other matrix effects. Therefore, ICP-AES does not always meet the requirements modern science and technology. The combination of ICP-AES with electrothermal evaporation of the sample (ETI-ICP-AES) significantly expands the capabilities of the method. By optimizing the pyrolysis and evaporation temperatures, analyte elements can be evaporated sequentially, separating them from the sample matrix. This method has the advantages of high sample introduction efficiency, the ability to analyze small sample quantities, low absolute detection limits, and the ability to directly analyze solid samples.

Analysis tools and conditions.An ICP generator with a power of 2 kW and a frequency of 27 ± 3 MHz was used; ISP burner; graphite furnace WF-1A; diffraction spectrometer RO5-2 with a diffraction grating of 1300 lines/mm with a linear dispersion of 0.8 nm/mm; pH meter Mettle Toledo 320-S; sedimentation centrifuge model 800.

Standard solutions and reagents.Stock standard solutions with a concentration of 1 mg/ml are prepared by dissolving the corresponding oxides (spectroscopic purity) in diluted HC1, followed by dilution with water to a given volume. A suspension of polytetrafluoroethylene was added to each standard solution to a concentration of 6% w/v.

We used Triton X-100 reagent grade (USA). The remaining reagents used were of spectroscopic grade; double distilled water. Titanium dioxide nanoparticles with a diameter of less than 30 nm.

Method of analysis.The required volume of solution containing metal ions is placed in a 10 ml graduated test tube and the pH is adjusted to 8.0 using 0.1 M HC1 and an aqueous solution of NH 3. Then 20 mg of titanium dioxide nanoparticles are added to the test tube. Shake the test tube for 10 minutes. (preliminary experiments showed that this is sufficient to achieve adsorption equilibrium). The tube is left for 30 minutes, then the liquid phase is removed using a centrifuge. After washing the precipitate with water, 0.1 ml of a 60% polytetrafluoroethylene suspension, 0.5 ml of a 0.1% agar solution, 0.1 ml are added to it. Triton X-100 and diluted with water to 2.0 ml. The mixture is then dispersed using an ultrasonic vibrator for 20 minutes to achieve homogeneity of the suspension before it is introduced into the evaporator. 20 μl of the suspension is added to the graphite furnace after heating and stabilization of the ICP. After drying, pyrolysis and evaporation, the sample vapor is transferred to the ICP by a current of carrier gas (argon); atomic emission signals are recorded. Before each sample injection, the graphite furnace is heated to 2700°C to clean it.

Application of the method.The developed method is used to determine Pb 2+in samples of natural lake water and river water. Water samples were filtered through a 0.45 µm membrane filter immediately after sampling and then analyzed.

1.4.2 Determination of lead combining real-time concentration followed by reversed-phase HPLC

Instruments and reagents. A diagram of the HPLC system with real-time concentration ("on-line") is shown in Fig. 1.1 The system consists of a Waters 2690 Alliance pump (in diagram 2), a Waters 515 pump (1), a Waters 996 photodiode array detector (7) , six-way switch tap (4), large volume injection device (holds up to 5.0 ml of sample) (3) and columns (5,6). The concentrating column was Waters Xterra™ RP 18(5 µm, 20 x 3.9 mm), Waters Xterra™ RP analytical column 18(5 µm, 150 x 3.9 mm). pH was determined with a Beckman F-200 pH meter, and optical density was measured with a Shimadzu UV-2401 spectrophotometer.

Fig 1.1Schematic of a real-time concentration system using a switch tap

All solutions were prepared using ultrapure water obtained using the Milli-Q50 Sp Reagent Water System (Millipore Corporation). A standard solution of lead (P) with a concentration of 1.0 mg/ml, working solutions with an ion concentration of 0.2 μg/ml are prepared by diluting standard ones. Use tetrahydrofuran (THF) for HPLC (Fisher Corporation), pyrrolidine-acetic acid buffer solution with a concentration of 0.05 mol/L. Before use, glassware was soaked for a long time in a 5% nitric acid solution and washed clean water.

Experimental technique. The required volume of a standard solution or sample is added to a 25 cm volumetric flask. 3, add 6 ml of solution T 4CPP with a concentration of 1 x10 -4mol/l in THF and 4 ml of pyrrolidine-acetic acid buffer solution with a concentration of 1 x10 -4mol/l and pH 10, dilute to the mark with water and mix thoroughly. The mixture is heated in a boiling water bath for 10 minutes. After cooling, dilute to the THF mark for subsequent analysis. The solution (5.0 ml) is introduced into the dispenser and sent to a concentrating column using mobile phase A at a speed of 2 cm3/min. Upon completion of concentration by eliminating the six-way valve, metal chelates with T 4CPPs adsorbed at the top of the concentrating column are eluted with a flow of mobile phases A and B at a rate of 1 ml/min in the opposite direction and sent to the analytical column. The three-dimensional chromatogram was recorded in the wavelength range of maximum absorption 465 nm using a detector with a photodiode array.

1.4.3 Stripping voltammetric determination of lead using a glassy carbon electrode system

Instruments and reagents.For the studies, we used an electrode system, which was an assembly of three identical glassy carbon (GC) electrodes (indicator, auxiliary, comparison) pressed into a common tetrafluoroethylene body. The length of each electrode protruding from the housing is 5 mm. The surface of one of them, chosen as an indicator, was electrochemically treated with an asymmetric current at densities in the range of 0.1-5 kA/m 2recommended for metals. The optimal surface renewal time was found experimentally and was 10-20 s. The indicator electrode served as the anode, and the stainless steel electrode served as the cathode. We used 0.1 M aqueous solutions of acids, salts, alkalis, as well as 0.1 M solutions of alkalis or salts in a mixture of organic solvents with water in a ratio of 1: 19 by volume. The condition of the treated surface was observed visually using a Neophot 21 microscope with an increase of about 3000.

Method of analysis.After processing, the electrode assembly was used to determine 3*10 -6M lead (II) by stripping voltammetry against a background of 1*10 -3M HNO 3. After electrolysis at – 1.5 V for 3 min with stirring with a magnetic stirrer, a voltammogram was recorded on a PA-2 polarograph. The potential of the lead anodic peak remained constant and amounted to - 0.7 V. The linear potential scan rate was 20 mV/s, the scan amplitude was 1.5 V, the current sensitivity was 2 * 10-7 A/mm.

Aqueous solutions of LiNO 3, NaNO 3, KNO 3as a processing electrolyte, they allow one to obtain stable heights already in the second measurement with satisfactory reproducibility (2.0, 2.9 and 5.4%, respectively). The greatest sensitivity of readings is achieved when using an electrolyte having a smaller cation.

1.4.4 Atomic absorption determination of lead by dosing suspensions of carbonized samples using Pd-containing activated carbon as a modifier

Analytical measurements were carried out on a SpectrAA-800 atomic absorption spectrometer with a GTA-100 electrothermal atomizer and a PSD-97 autosampler (Varian, Australia). We used graphite tubes with pyrocoating and an integrated platform (Varian, Germany), hollow cathode lamps for lead (Hitachi, Japan) and cadmium (C Varian, Australia). Integral absorption measurements with correction for nonselective light absorption (deuterium system) were carried out at a spectral slit width of 0.5 nm and a wavelength of 283.3 nm. Argon "highest grade" served as a shielding gas. The temperature program for the atomizer operation is given in Table 1.1

Table 1.1 Temperature program for the operation of the electrothermal atomizer GTA-100

StageTemperature,°CDrying 190Drying 2120Pyrolysis1300Cooling50Atomization23OOCleaning2500

Palladium-containing compositions based on activated carbon and carbonized hazelnut shells were studied as modifiers for the atomic absorption determination of Pb in a graphite furnace. The metal content in them was 0.5-4%. To assess the changes occurring with the components of the synthesized modifiers under reducing conditions implemented during the analysis, the materials were treated with hydrogen at room temperature.

A solution with a known concentration of Pb was prepared by diluting GSO No. 7778-2000 and No. 7773-2000 with 3% HNO 3. The concentration range of working standard solutions of the element for constructing calibration dependencies was 5.0-100 ng/ml. Deionized water was used to prepare solutions .

When constructing pyrolysis and atomization curves, we used both a standard solution of the element and a carbonized “Standard sample of the composition of ground wheat grain ZPM-01”. In the first case in plastic cup autosampler was mixed with 1.5 ml of a standard solution of the element (50 ng/ml Pd in 5% HNO 3) and 10-12 mg of palladium-containing activated carbon; the suspension was homogenized and dosed into a graphite furnace. In the second, the same amount of modifier was added to the prepared suspension of carbonized sample (5-10 mg of sample in 1-2 ml of 5% HNO3 ).

1.4.5 Photometric determination and concentration of lead

Lead acetate of analytical grade was used in this work. The compounds (Fig. 1, which are dibasic acids) were obtained by azo coupling of a solution of 2-hydroxy-4 (5) - nitrophenyldiazonium chloride and the corresponding hydrazone. Solutions of formazans in ethanol were prepared by precise weighing.

The optical density of solutions was measured on a Beckman UV-5270 spectrophotometer in quartz cuvettes (l = 1 cm). The concentration of hydrogen ions was measured using an I-120M ion meter.

The reagents react with lead ions, forming colored compounds. The bathochromic effect during complex formation is 175 - 270 nm. Complexation is influenced by the nature of the solvent and the structure of the reagents (Fig. 1).

The optimal conditions for the determination of lead are a water-ethanol medium (1:

) and pH 5.5-6.0, created by an ammonium acetate buffer solution. The detection limit for lead is 0.16 µg/ml. Analysis duration 5 min.

The most interesting is the use of formazan as a reagent for the concentration and subsequent photometric determination of lead. The essence of the concentration and subsequent determination of lead (II) using formazan is that the lead complex is extracted from a water-ethanol solution in the presence of Ni, Zn, Hg, Co, Cd, Cr, Fe ions with a chloroform solution of formazan.

For comparison, we used the method for determining lead with sulfarsazen (GOST, MU issue 15, No. 2013-79). The results of the analysis of model solutions using two methods are given in Table 1.2 Comparison of variances using the F-criterion showed that Fexp< Fтеор (R= 0.95; f 1=f 2= 5); This means that the variances are homogeneous.

Table 1.2 results of determination of lead in model solutions (n=6; P=0.95)

Introduced, µg/mlFoundFoundFexpF theorsulfarsazen, µg/mlS r formazan, µg/mlS r 4.14 2.10 3.994.04 ±0.28 2.06±0.29 3.92 ±0.17 0.29 3.92 ±0.172.8 5.5 1.74.14 ±0.07 2.10 ±0.08 3.99 ± 0.072.1 *10 -2 2.5*10-2 2.1*10-23.97 3.57 3.374.53

2. Experimental part

Measuring instruments, reagents and materials:

When performing this method, the following measuring instruments, devices, reagents and materials are used:

· Atomic absorption spectrometer

· Spectral lamp with hollow cathode

· Compressor for supplying compressed air

· Gearbox - according to GOST 2405

· Laboratory beakers, capacity 25-50 cm3 - according to GOST 25336

· Measuring flasks of the second accuracy class with a capacity of 25-100 cm3

· Laboratory funnels according to GOST 25336

· Distilled water

· Concentrated nitric acid, x. h., GOST 4461-77

· Standard lead solution (c = 10-1 g/l)

Determination conditions:

§ Wavelength when determining lead? =283.3 nm

§ Monochromator slit width 0.1 nm

§ Lamp current 10 mA

Method of measurement:

Atomic absorption spectroscopy is based on the absorption of radiation in the optical range by unexcited free lead atoms formed when the analyzed sample is introduced into a flame at a wavelength ? =283.3 nm.

Safety requirements:

When performing all operations, it is necessary to strictly observe the safety rules when working in a chemical laboratory, corresponding to GOST 126-77 "Basic safety rules in a chemical laboratory", including rules safe work with electrical devices with voltages up to 1000 volts.

Preparation of lead calibration solutions:

Solutions are prepared using a standard lead solution with a concentration

c= 10-1 g/l.

To construct a calibration curve, use solutions of the following concentrations:

*10-4, 3*10-4, 5*10-4, 7*10-4, 10*10-4g/l

Standard solution with a volume of 10 cm 3add to a 100 ml flask and fill to the mark with distilled water. In 5 volumetric flasks with a capacity of 100 ml add 1, 3, 5, 7, 10 ml of intermediate solution (solution of concentration 10 -2g/l). Make up to the mark with distilled water. Construct a gradation graph in coordinates A, y. e from s, g/l

Table 2.1 Measurement results

concentration, g/lSignal, u. e. 0.000130.0003150.0005280.0007390.001057

Sample preparation:

I take a sample of coffee weighing 1.9975 g.

I add it to a 100 ml glass.

I dissolve the sample in 20 ml of concentrated nitric acid.

I evaporate the contents of the glass in a water bath to half the original volume, stirring occasionally.

The solution in the beaker after evaporation is cloudy, therefore, using a laboratory funnel and a paper filter, I filter the contents of the beaker into a 25 ml beaker.

I add the filtered solution into a 25 ml flask and bring it to the mark with distilled water.

I thoroughly mix the contents of the flask.

I add part of the solution from the flask into a pipette, which serves as a sample to determine the lead content.

To determine an unknown concentration, the solution is introduced into the atomizer and after 10-15 seconds the readings of the device are recorded. The average readings of the device are plotted on the ordinate axis of the calibration graph, and the corresponding concentration value, сх g/l, is found on the abscissa axis

To calculate the concentration in the sample, I use the calculation formula:

С =0.025*Сх*10-4*1000/ Мnav (kg)

Table 2.2 Measurement results

ProbaSignal, u. e. AverageC X , g/l 123 coffee15141514,666672.9*10 -4cheese00000apples juice00000grape juice00000cream3222.333337.8*10 -5water00000shampoo00000

Based on the tabular data, I calculate the concentration of lead in the samples:

Sample MPC, mg/kg coffee 10 cream

C (Pb in coffee sample) = 3.6 mg/kg

C (Pb in cream sample) = 0.98 mg/kg

conclusions

The work describes methods for determining lead using various physical and chemical methods.

Sample preparation methods for a number of food objects are presented.

Based on literature data, the most convenient and optimal method for determining lead in various food products and natural objects was selected.

The method used is characterized by high sensitivity and accuracy, along with the absence of a response to the presence of other elements, which allows one to obtain true values ​​​​of the content of the desired element with a high degree of reliability.

The chosen method also makes it possible to conduct research without any particular difficulties in sample preparation and does not require masking of other elements. In addition, the method allows you to determine the content of other elements in the test sample.

Based on the experimental part, we can conclude that the lead content in Black Card coffee does not exceed the maximum permissible concentration, therefore the product is suitable for sale.

List of used literature

1. Glinka N.I. General chemistry. - M.: Nauka, 1978. - 403 p.

Zolotov Yu.A. Fundamentals of analytical chemistry. - M.: Higher. school; 2002. - 494 p.

Remy G. General chemistry course. - M: Ed. foreign lit., 1963. - 587 p.

GOST No. 30178 - 96

Yiping Hang. // Journal. analyte khim., 2003, T.58, No. 11, p.1172

Liang Wang. // Journal. analyte khim., 2003, T.58, No. 11, p.1177

Nevostruev V.A. // Journal. analyte khim., 2000, T.55, No. 1, p.79

Burilin M.Yu. // Journal. analyte khim., 2004, T.61, No. 1, p.43

Maslakova T.I. // Journal. analyte khim., 1997, T.52, No. 9, p.931

METHODOLOGICAL INSTRUCTIONS
FOR PHOTOMETRIC DETERMINATION OF LEAD IN AIR

APPROVED by Deputy Chief State Sanitary Doctor of the USSR A.I.3aichenko on June 6, 1979 N 2014-79

I. General part

1. The determination is based on the colorimetric determination of colored solutions formed by the reaction of lead ion with xylenol orange.

2. Sensitivity of determination - 1 μg in the analyzed volume of solution.

3. The determination does not interfere with iron, aluminum, coal dust, silicate dust containing aluminum and iron, quartz, tin and antimony.

4. The maximum permissible concentration of lead in the air is 0.01 mg/m.

II. Reagents and equipment

5. Reagents and solutions used.

Basic standard solution containing 100 µg/ml. 0.0183 g Pb (CHCOO). 3 HO are dissolved in acetate buffer with pH = 6 in a 100 ml volumetric flask and adjusted to the mark with acetate buffer, shelf life 1 month.

A standard solution N2 containing 10 µg/ml of lead is prepared before use by appropriately diluting the original solution.

Buffer mixture pH=5.8-6.0; sodium acetate 0.2 M - 9?..* ml, acetic acid 0.2 M - 6 ml.
________________

Xylenol orange, indicator, TU 6-09-1509-72, analytical grade. 0.01% solution (initial 100 mg/100 ml). Shelf life: 7 days, store in a closed bottle.

The working solution of xylenol orange is prepared by diluting the main (initial) solution 10 times before analysis.

6. Utensils and utensils used.

Aspiration device.

Cartridges for filters.

Chemical test tubes with a height of 150 mm and an internal diameter of 15 mm.

Volumetric flasks, GOST 1770-59, with a capacity of 25 and 100 ml.

Graduated pipettes, GOST 1770-59, with a capacity of 1, 2 and 5 ml.

Chemical glasses with a capacity of 25 ml.

Sand bath.

Photoelectric colorimeter FEK-?..*-57 or SF-10.
________________
* Defect of the original. - Database manufacturer's note.

Filters AFA-VP-20.

III. Air sampling

7. Air is aspirated at a speed of 20 l/min through an AFA-VP-20 filter placed in a plexiglass cartridge. For analysis, 300 liters of air should be taken.

IV. Definition description

8. Before analysis, it is necessary to check the cleanliness of the dishes as follows: are the dishes rinsed after washing?..* ml of distilled water with 1 ml of 0.01% xylenol orange. The color should be yellow. When the yellow color of the solution turns purple, the dishes must be washed again as follows: with water, acetate buffer, again with water, distilled water.
________________
* Defect of the original. - Database manufacturer's note.

The filter with the sample is transferred in an unfolded state to a funnel D = 7 cm and the sample is treated with 5 ml of glacial acetic acid. In this case, the precipitate is dissolved with simultaneous filtration through the same filter. The filter is washed with 5 ml of distilled water, the filtrate is collected in a glass beaker with a capacity of 40-50 ml and evaporated in a sand bath at a temperature of 160-190° to a dry residue. The dry residue is dissolved in 4 ml of acetate buffer, 1 ml of 0.01% xylenol orange is added and after 10 minutes the optical density of the solutions is measured on a photoelectrocolorimeter at a wavelength of 536 nm in a cuvette with a layer thickness of 10 mm.

For quantitative determination, construct a calibration graph of the dependence of the optical density of the standard scale on the concentration of lead in the solution.

Table 10

Standard scale

Standard number		Standard solution N 2, ml	Acetate buffer, ml	Xylenol orange, ml

Pages:

UDC 543.(162:543 42:546.815

HER. Kostenko, M.G. Christiaisen, E.N. Butenko

PHOTOMETRIC DETERMINATION OF MICRO QUANTITIES OF LEAD IN DRINKING WATER USING SULPHONASE III

The complexation of Pb(P) with sulfonase III was studied and, based on the data obtained, a method for the photometric determination of lead in drinking water after preliminary extraction concentration in the form of a complex with dithi:un was developed.

The problem of environmental purity of raw materials has great importance for the production of food products. Therefore, quality control of drinking water, as one of the main components of various drinks, is very important, and the creation of new selective, sensitive and rapid methods for the photometric determination of toxic metals is quite relevant. Among the latter, one of the most dangerous to human health is lead. The value of its maximum permissible concentration in various food items is 0.1 - 10 mg/kg, and in drinking water - 0.03 mg/dm3.

Quite a number of organic reagents have been proposed for the photometric determination of lead. The main characteristics of the methods are given in table.J.For the most part, these methods are not selective enough. Therefore, the standard method for determining lead in drinking water involves its preliminary extraction in the form of a complex with dithizone. Then, during strip extraction, sulfarsazene is added and the optical density of the complex is measuredPb(II) with this reagent,

Reagent bis-sulfone or sulfonazo III (SFAZ.HSR)used to determine small amounts of gallium, scandium, indium and barium - / .

Molar ratioPb(II) - SFAZ in the complex (equal to 1:1) is confirmed by the constancy of the value of the constant K under different conditions for its determination (Table 2).

Complex concentration values ​​required for calculationsPbH2R:under equilibrium conditions was determined by the equation

= (A-ekCr-0 / (єк - eR)■ I,

Where }