Security in Water Analysis

Rahul C. DeshpandeWater & Food AnalyticsMerck Millipore

Water - Do we have enough ?

Challenges…. Water becoming Scarce… Pollution a global issue Availability of safe water Water Quality Monitoring

Today one-fifth of world does not have access to safe drinking water.

Population Explosion & per capita consumption of water will increase

Water Crisis of Unusual Dimensions within 2 decades…

Subsidized prices of water incline consumers to use water liberally, leading to considerable waste.

Water – The World Perspective

It is indeed a Concern…

Situation in South Asia ( India / Nepal / Bangladesh / Srilanka )

By 2025 the population would be crossing 1.6 Billion. People in urban areas would cross @ 40 % , currently @ 25 % Demand for potable water would thus go UP…

Source: International Conference On Water Quality Management

Initiatives!!

Authorities ( PCB / Environmental Ministry) Set up Regulations

Academia / Research Study / Awareness

Industry Waste Water Treatment plants

Technology provides Latest techniques – reduction of waste Recycle / Re – use

Based on studies

Laboratory analysis

Data creation

Where & How was the Analysis done ??Precision / Robustness / Validation Reliability

Challenges – to get Reliable Data ….

Changing Analytical NEEDS ...Today…Tomorrow..

Innovative productSimplicity in operation

Do we have a RELIABLE partner who can provide SECURITY ??

Meets Specification

Compliance to Regulations

Reproducibility in results

Documentation

Cost Effective technique

Time Management

Water Analysis Microbial Analysis Quality Assurance / Control In Process Control Waste Water laboratory …

Complete Solution !!!!

Typical Sources of “errors”

Manpower ( Operator effect )

Materials

- sample effect (homogeneity, stability of the sample, etc.)

- consumables (reagents, products, reference standard solutions), Matrix

Validation procedure and ISO 17025 accreditation

Equipment / Machines;- Effect of the apparatus (response, sensitivity, integration mode)- Laboratory equipment (balance, glassware , instruments);

Method being used- Application effect of the procedure - operating conditions, successive operations,- no. of measurements, data processing

Ambient conditions- temperature, pressure, lighting, vibration, radiation, humidity

2.8 Quality of ChemicalsThe quality of chemicals/solvents used in the analytical laboratory may varyfrom laboratory grade to Analytical or Guaranteed Grade [ Analar or AR orG.R.). The quality of chemical/solvents may become one of the causes ofanalytical errors may affect the analytical instrument or may lead tointerferences during determinations. Hence, selection of laboratory chemicals of an appropriate quality is most important factor for achieving result with desired accuracy.For preparation of all standard solutions only “Analytical reagent grade (AR)or guaranteed reagent grade (GR) should be used, since their purity levelsare known. Reference Materials (RM’s) or Certified Reference Materials(CRM’s) should be used for calibrations during analysis of metals, pesticides, and other organics such as THM, PAH’s, BTX etc.

Source :Guidelines - EPA act ,1986

Typical Sources of “errors” during Analysis (Chemicals used )

Table 3.5: Collection and Preservation of Environmental Samples

Typical Sources of “errors” during Analysis

Source :Guidelines - EPA act ,1986

Why Sample preparation

Sample preparation means transferring the analyte to a status where the chosen method works

Without any exception, all analytical techniques require ideal sample conditionsaccording to the measuring procedure used

Turbid solutions (suspended particles) / dissolved salts High concentrations of dissolved or suspended organic compounds

Samples contain complexing agents (EDTA, Organophosphonic acid)

pH shift / colored additives that may disturb the photometric determination

Sample with high concentrations of oxidizing and reducing compounds

Detection of copper in waste water samples

Filtration Filtration Homogenization

DigestionDigestion

Dissolved part =

Cu2+ ions+

Cu-EDTA complexes+

Solid substances, e.g. Cu(OH)2

Dissolved part =

Cu2+ ions+

Cu-EDTA complexes

Dissolved part =

Cu2+ ions

Sample Preparation Techniques Homogenization is performed 2 min at 5000 – 20000 rpm, a sample is

taken while stirring

Required for the determination of

- Total phosphorus / Total nitrogen- COD, BOD, TOC\

Colour Removal by means of activated charcoal

May lead to a partial or complete loss of the analyte

Occurs for cations, that easily generate hydroxides such as metals:

- Iron, copper, chrome, zinc, nickel, manganese, lead, cadmium

Digestion

For Organic compounds that disturb the determination

Complexing agents / Colour Additives / Turbid Samples

Sample

Right Sample Preparation – the KEY

Persulfatedigestion

Aqua regiadigestion

Hydrochloric aciddigestion

Sulphuric acid/H2O2

digestion

Filtration

Discoloration

Dilution

Carrez clarification

Homogenization

pH value

Challenges in a Laboratory Today …….

Changing Analytical NEEDS ...Today…Tomorrow..

Innovative productSimplicity in operation

This is where steps in…

Meets Specification

Compliance to Regulations

Reproducibility in results

Documentation

Cost Effective solution

Time Management

Water Analysis Microbial Analysis Quality Assurance / Control In Process Control Waste Water laboratory …

Parameter Limit

pH 6.5 - 8.5

BOD (3 days at 27oC) 50

Phenol** 5

Sulphide as S 2COD 250

Cyanide as CN0. 2

Fluoride as F*** 15

Total suspended solids 100

Chromium****

Hexavalent 0.1

Total 2

Waste Water Analysis

Industry Specific Requirement

Spectroquant® PharoThermoreactor TR series MultiParamater Instrument 340 IOxitop® – BOD Analysis

Measurement of Oxygen Demand (COD)

How to measure COD Introduced Measuring Chloride Temp TimeMethods last update ranges tolerance

Open refluxion and titration

– ISO 6060 1989-11 30 to 700 mg/l 1000 mg/l 148 ± 3°C 10 + 110 min

– APHA 5220 B 21th ed 50 to 900 mg/l no information - 2h

– EPA 410.2 1978 5 to 50 mg/l no information - 2h

– EPA 410.1 1978 > 150 mg/l 2000 mg/l - 2h

– EPA 410.3 1978 250 to 800 mg/l 4000 to 20000 mg/l - 2h

– DIN 38409 H41-1 1980-12 15 to 300 mg/l 1000 mg/l 148 ± 3°C 10 + 110 min

– DIN 38409 H43-1 1981-12 15 to 300 mg/l 1000 mg/l - 5 + 15 min

– DIN 38409 H44-1 1992-05 5 to 50 mg/l 300 mg/l 152 ± 3°C 2h

Closed refluxion and titration

– APHA 5220 C 21th ed 40 to 400 mg/l no information 150 ± 2°C 2h

– ISO 15705 2002-11 to 1000 mg/l 1000 mg/l 150 ± 5°C 2h ± 10 min

Photometric analysis

– ISO 15705 2002-11 to 50 mg/l 1000 mg/l 150 ± 5°C 2h ± 10 min

– ISO 15705 2002-11 to 150 mg/l 1000 mg/l 150 ± 5°C 2h ± 10 min

– ISO 15705 2002-11 to 1000 mg/l (1500 mg/l) 1000 mg/l 150 ± 5°C 2h ± 10 min

– APHA 5220 D 21th ed to 90 mg/l no information 150 ± 2°C 2h

– APHA 5220 D 21th ed 100 to 900 mg/l no information 150 ± 2°C 2h

– EPA 410.4 1978 20 to 900 mg/l no information 150°C; 2h

– EPA 410.4 1993-08 3 to 900 mg/l no information 150°C; 2h

Analysis made simple - Spectroquant® System

Pre Treated Sample + Chemistry( Colour Development )

Spectroquant® Photometer / Spectrophotometer

Secure Reliable / Traceable Validated Results

COD Analysis ( 4.00 mg/l up to 90,000 mg/l ) ( 9 Ranges)

COD Analysis

COD is the single largest parameter used across the industry …. Metal / Heavy Metal Analysis specific to the industry

Waste volume

Mercury-sulphate

Silver-sulphate

Potassium-dichromate

Sulphuricacid

COD Cell testMerck 1.14540

COD Standard method ISO 6060 (open reflux, titrimetric)88 mg 21 mg 6 mg 3.1 ml 6 ml

800 mg

300 mg

58.8 mg 31 ml

130 ml

Thermoreactor TR 320 – 12 Samples Thermoreactor TR420 – 24 Samples Thermoreactor TR 620 – 12 X 12 Samples

ISO conformity of Merck COD Cell Tests

AQA – Analytical Quality Assurance

100 % Fascinated by Analytics

Complete - Analytical Quality Assurance

+++++++++++++++++++++++++++++++

AQA 1 Checking the photometer –PhotoCheck / CertiPUR UV/VIS standards. AQA 2 Check - complete system [instrument + test kit + pipette + operator] CombiCheck, dilutedstandard solutions (CRM), CertiPUR standard solutions.

AQA 3 Influence of sample [matrix check]Multiple spiking & dilution (CombiCheck )

Focus Products :

CombiCheck®PipeCheck® Spectroquant ®Reference Standard

PhotoCheck®CertiPUR®

Standard SolutionsCRM

Waste disposal advice

Merck Millipore A part of Merck KGaA a global pharmaceutical and chemical company with a rich history that began in 1668 ( 343 Years) with a presence in over 60 countries.

Merck Millipore focuses on high-quality and innovative products to support ,analytical needs in applications ranging from R & D / Quality Control / Healthcare

InnovationNew products with cutting edge technology ensuring continues suitability & protection to the environment.

Association :Partnership with Global agencies UNICEF , WHO, Environmental Protection Agency in providing solutions for drinking / waste water

Experience :Decades of cooperation with Central & state bodies , In laboratory set up ( Water Quality Monitoring ) for mega city & rural water projects across India -Training needs / Service support

WnFA : - Objective

To Provide Analytical Solutions for the ..Water Market World Wide

Thanks !!!

“Quality is never an accident .... It is always the result of high intention, sincere efforts , intelligent direction & skillful execution ...... ………….. It represents the wise choice of many alternatives “--William A Foster