W101 - The Impact of reliable measurements on the ...

© NMISA 2012

The impact of reliable

measurements on the protection

of the environment on a global

scale

Wynand LouwDirector of Technical Infrastructure DevelopmentObo of the CEO of NMISA

© NMISA 2012

Outline of Talk

� Accurate and Reliable Measurement

� Measurement in the Environment: Greenhouse Gases, Ozone, VOCs

� The NMISA and Environmental Analysis

© NMISA 2012

Why Accurate Measurement?

A. Economic reasons

Economic externalities e.g. regulations that protect the

citizen

Assessment of the added value provided by an innovation

Specification of products and services for trade

Quality control or improvement in the efficiency of manufacturing

processes

Mea

sure

men

t Im

pact

s th

e E

cono

my

in fo

ur

way

s

© NMISA 2012


B. Food Safety and Health

Safety from Farm to Fork

Scandals

-dioxin in milk-glycol in wine-BSE in beef

Treaties and

Directives

Environment

© NMISA 2012

Environmental Measurements

Soil and water

Air Quality

Pollutants

Atmospheric Parameters

© NMISA 2012


• Treatment of seeds and plants• Animal feed (natural and

industrial)• Treatment of animals (treatment

for sickness, hormones)• Industrial food processing• Storage, transport, sales,

delivery conditions• Nutritional values

© NMISA 2012


C. Law enforcement and Health

• Forensics• Speed trapping• Blood alcohol levels• Diagnostics and Dosimetry• Trade/Legal metrology

© NMISA 2012

What is Accurate Measurement?

Accuracy and Precision

• the accuracy of a measurement system is the degree of closeness of measurements of a quantity to that quantity's actual (true) value

• The precision of a measurement system, also called reproducibility or repeatability is the degree to which repeated measurements under unchanged conditions show the same results

• A measurement system can be accurate but not precise, precise but not accurate, neither, or both

© NMISA 2012

What is Accurate, Reliable Measurement?

© NMISA 2012

What is Traceability?

A measurement system is designated valid if it is both accurate and precise

How is it achieved?

Through measurement standards compared to a common artefact or physical constant of nature

through primary realisation of a unit

© NMISA 2012

The Constants and Measurement Units

A. Some known natural, constant, material phenomenon is produced under well controlled experimental conditions and a well-accepted value (and uncertainty) is assigned to a well known property of that phenomenon

B. This is then used as an “etalon” for the appropriate quantity, to create and calibrate a measurement scale

© NMISA 2012

Consumer assurance

Scale, balance or standard weights are calibrated by accredited cal

labs in SA against calibrated mass pieces

Mass Measurement in Shop SA

Mass Measurement in Shop X

NMISAMass pieces from accreditedcal lab is calibrated against

the national kilogram SA

NMIXMass pieces from accreditedcal lab is calibrated against

the national kilogram X

The copies of the prototype, the “National kilograms” are compared to the protoype Kg

at the BIPM

Scale, balance or standard weights are calibrated by accredited cal

labs in X against calibrated mass pieces

Measurement equivalence achieved

Legal Metrology (NRCS) ensures

compliance through inspection

SANAS ensures competency

through accreditation

NMISA ensures traceability through the

NMS

The Last Artefact unit

© NMISA 2012

The Temperature Scale

The unit of the fundamental physical quantity known as thermodynamic temperature, symbol T, is the kelvin, symbol K, defined as the fraction 1/273.16 of the thermodynamic temperature of the triple point of water

The ITS-90 extends upwards from 0.65 K to the highest temperature practicably measurable in terms of the Planck radiation law using monochromatic radiation.

T90/K t90/°C Substance

3 to 5 -270.15 to -268.15 He

83.8058 -189.3442 Ar

302.9146 29.7646 Ga

933.473 660.323 Al

1357.77 1084.62 Cu

© NMISA 2012

Metre Convention

1875

International Committee for Weights and Measures (CIPM)

Consists of 18 individuals elected by the CGPM

It is charged with supervision of the BIPM and affairs of the Metre Convention

The CIPM meets annually at the BIPM

General Conference on Weights and Measures (CGPM)

meets every four years and consists of delegates from Member States

International Bureau of Weights and Measures

(BIPM)

International Centre for metrology

Laboratories and offices at Sévres (Paris)

Diplomatic treaty

International organisations

National metrology institutes (NMIs)

Governments of Member

States

Consultative Committees (CCs)

Ten CCs normally chaired by a member of CIPM; to advise the CIPM, act on

technical matters and take important role in CIPM MRA; representatives of

NMIs and other experts

Associate States and

Economies of the CGPM

CIPM

MRA

© NMISA 2012

The RMO Comparison structure

© NMISA 2012

Standards and Scales for the Monitoring of Global Greenhouse Gases and other Trace Species

In consultation with Head of Chemistry BIPM:

R.I. Wielgosz

([email protected])

16Bureau International des Poids et Mesures

© NMISA 2012

Outline

� Greenhouse Gases and World Metreological Organisatio n(WMO)- Global Atmospheric Watch (GAW) variables

� Definitions

� WMO Scales and traceability chain

� CO2� CH4� N2O� O3� VOCs� Other species

© NMISA 2012

WMO-BIPM Collaboration (1)

� 1999, Resolution 4 of the 21st CGPM on use of SI units in studies of Earth resources, the environment (initial driver from BIPM's Consultative Committee for Photometry and Radiometry)

� 2000, BIPM Laboratories start gas metrology programme in collaboration with NIST for international equivalence of standards for Tropospheric Ozone

� 2001, BIPM's GAWG experts attend the 2001 WMO-GAW meeting

� 2002, Working agreement agreed between BIPM and WMO (following meeting of WMO Executive Council)

© NMISA 2012


� 2003, WMO-GAW participate in CCQM-P41 on greenhouse gases (carbon dioxide and methane) (NOAA (US) and CSIRO (Australia))

� 2003-2005 WMO-GAW's World Calibration Centre for Surface Ozone (EMPA, CH) participate in comparison on surface ozone (CCQM-P28)

� 2005 BIPM's CCQM Gas Analysis Working Group Experts participate in WMO-GAW 2005 meeting

� 2006 WMO-GAW-VOC expert group requests NMIs active in CCQM GAWG group to develop gas standards and act as a Central Calibration Laboratory (CCL) for WMO-GAW (including VOCs and formaldehyde)

© NMISA 2012


� 2008, Expert National Metrology laboratories in BIPM's CCQM Gas Analysis group complete international comparison on VOCs, the technical basis for the establishment of a CCL for VOCs in WMO-GAW

� 2007-2009, Request from WMO-GAW's Surface Ozone and Surface Radiation Central Calibration laboratories for WMO to sign the CIPM-MRA so that they can participate in BIPM's series of Key Comparisons

� 2009, BIPM laboratory experts to participate in WMO-GAW workshop on Ozone and WMO-GAW 2009

� 2010, WMO-BIPM workshop on “Measurements Challenges for Global Observation Systems for Climate Change Monitoring’’

© NMISA 2012

Definitions (WMO) [1]

Central Calibration Laboratory (CCL)

Within the WMO/GAW network, laboratory responsible for maintaining thestandard scale for the species under consideration.

Conventional reference scale (reference-value scale , standard scale)

for particular quantities of a given kind, an ordered set of values,continuous or discrete, defined by convention as a reference for arrangingquantities of that kind in order of magnitude

NOTES1) The scale is based upon a number of primary standards and a measurement procedure to

interpolate other values.2) Within WMO/GAW, the conventional reference scale refers in particular to the calibration

scale used within the GAW network. In the case of CO2, CH4, N2O and CO, this scale is implemented as a family of gas cylinders maintained at the CCL (NOAA).

© NMISA 2012

Definitions (WMO) [2]

Primary standard

Standard that is designated or widely acknowledged as having the highestmetrological qualities and whose value is accepted without reference toother standards of the same quantity

NOTES1) In particular with respect to trace gases, standard with assigned mole

fraction based on absolute calibration, i.e. gravimetric or equivalent method.2) Within WMO/GAW, the primary standards for CO2, CH4, N2O and CO are

maintained at NOAA.

World Calibration Centre (WCC)

Part of the GAW network, responsible for quality assurance measures forone or more components, by way of audits and comparisons

NOTEFor each component under consideration, the WCC refers to the calibrationscale maintained by the CCL designated by GAW.

© NMISA 2012

Climate Change – Global Warming

Source: IPCC 4th Report WG1

© NMISA 2012

Greenhouse Gases

� Drivers and Requirements

Bureau International des Poids et Mesures

Climate Change

Monitoring of Greenhouse Gases

[Intergovernmental Panel on Climate Change (IPCC), 2001]

© NMISA 2012

Climate Change – Greenhouse Gases

Global average abundances of the major, well-mixed, long-lived greenhouse gases - carbon dioxide, methane, nitrous oxide, CFC-12 and CFC-11 - from the NOAA global air sampling network

© NMISA 2012

Calculation of Global Average CO2 Concentrations (1)

1) WMO-GAW network supplies CO2 and CH4 data of theGlobal Climate Observing System (GCOS)

2) World Data Centre for Greenhouse Gases (WDCGG) – JMACalculates global mean mole fractions

3) NOAA also publishes global mean values based on theirMeasurement network

© NMISA 2012

CO2 Global mapping

© NMISA 2012

WMO-GAW Network for Carbon Dioxide

© NMISA 2012


WDCGG Global Analysis Method

Step 4: Abstraction of a station’s average seasonal variation expressed by the Fourier polynomial

Step 5: Interpolation for data gaps

Step 6: Extrapolation for synchronization of data period

Step 7: Calculation of the zonal and global mean mole fractions, trends, and growth rates.

Step 1: Station selection based on traceability to the WMO standard scale

Step 2: Integration of parallel data from the same station

Step 3: Selection of stations suitable for global analysis

© NMISA 2012


Long term trend and average seasonal variation

Monthly variations of zonally averaged CO 2mole fractions

Source: WMO/TD-No. 1473, Technical Report of Global Analysis Method for Major Greenhouse Gases by the WDCGG

© NMISA 2012


Difference between WDCGG and NOAA globally-averagedCO2 monthly mole fractions

Major cause for differences is use of different mon itoring stations, rather than differences in calculation me thods

Source: WMO/TD-No. 1473, Technical Report of Global Analysis Method for Major Greenhouse Gases by the WDCGG

© NMISA 2012

WMO-GAW Data Quality Objectives

Source: WMO/TD-No. 1487, 14th WMO/IAEA Meeting of Experts on Carbon dioxide, other Greenhouse Gases and Related Tracers Measurement Techniques (2007)

© NMISA 2012

Mole fraction of CO2 in airSI-Unit: µmol/mol

WMO-GAW (Metrological) Traceability Chain

Secondary Standards

Laboratory Standards

Transfer Standards

Working standards

NDIR Calibration Procedure

Atmospheric Sample

RESULTCO2 in µmol/mol


Primary

reference

measurement

procedure

Primary

standards

Secondary

calibrator

15 CO2-in-air primary standards

(WMO CO2 Mole fraction Scale )

NOAA Manometric procedure

GAW Station

measurement

procedure and

standards




Reference Gas

u(x)

0.069 µmol/mol

0.070 µmol/mol

0.071 µmol/mol

0.072 µmol/mol

0.073 µmol/mol

© NMISA 2012

NOAA Manometric system for CO2 in Air Calibrations

C.L. Zhao et al., J. Geophys. Res., 102, 5885-5894 (1997)

© NMISA 2012

Manometric system for Absolute measurement of

CO2 concentration in Air

© NMISA 2012

Calibration Campaigns on WMO Scale Primary

Standards

u(xrep) = 0.03 µmol/mol

C.L. Zhao et al., J. Geophys. Res., 111, D08S09,(2006)

© NMISA 2012

Published uncertainty budget for Manometric System

u(xCO2)= Q[u(xrep), u(xSE)]

u(xCO2)= Q[0.03, 0.062] µmol/mol = 0.069 µmol/mol

C.L. Zhao et al., J. Geophys. Res., 111, D08S09,(2006)

© NMISA 2012

Uncertainty of subsequent value transfers/

calibrations

u(xNDIR)= 0.014 µmol/mol

u(xPS-CO2)= Q[0.069, 0.014] µmol/mol = 0.070 µmol/mol

u(xSS-CO2)= Q[0.070, 0.014] µmol/mol = 0.071 µmol/mol

Standard Calibration Interval Lifetime

Primary 2 years > 30 years

Secondary 0.5 years 3-5 years

Laboratory 2 years 20-30 years

Transfer 0.5 years 3-5 years

Working 0.25 years 0.25 years

Reference gas 0.25 years 0.25 years

© NMISA 2012

CCQM-P41, Carbon dioxide, 365 µmol/mol (2003)

WMO-GAW Laboratories

Agreement with gravimetric value

Comparison coordinated by NMi-VSL (NL)

© NMISA 2012

CCQM-P41, Carbon dioxide, 365 µmol/mol (2003)


DQO= ± 0.10 µmol/mol = ± 0.03%

© NMISA 2012

Commutability and Method Comparisons

1) CO2 in N2 standards not commutable with NDIR methods

- Effect as large as 5 µmol/mol

2) IDMS method developed; agreement within 0.52 µmol/mol(Verkouteren and Dorko (NIST), Anal. Chem., 61, 2416-2422, 1989)

3) Similar methods developed at NPL 1997 (Milton and Wang, International Journal of Mass SpectrometryVolume 218, Issue 1, 15 June 2002, Pages 63-73)

© NMISA 2012

Methane is the major greenhouse gas (18.2 % to the overall global

radiative forcing).

Before the industrial era ~ 700 ppb 2008 ~1797 ppb (7 ppb/year).

Figure 4. Globally averaged CH4 (a) and its growth rate (b) from 1984 to 2008.

Methane Ambient Levels (CCQM -K82)

CCQM-K82

Jointly coordinated by NIST and the BIPM

© NMISA 2012

CCQM-P41, Methane 1.8 µmol/mol (2003)

WMO-GAW Laboratories

1.7 % difference from gravimetric value (WMO Scale was CMDL83)


© NMISA 2012

WMO Scale for Methane (1)

1) NOAA04 has replaced CMDL83 as the WMO CH 4 scale

2) CMDL83 established in 1983 based on two CH 4 in air Standards, calibrated at the Oregon Graduate Instit uteagainst commercially prepared standards verified ag ainstNIST SRM-1659 (9.5 µmol/mol)

3) NOAA04 established in 2004 based on 16 gravimetr icallyPrepared standards (300-2600) nmol/mol

© NMISA 2012


16 gravimetrically produced CH 4 in air standards

E.J. Dlugokencky et al., J. Geophys. Res., 110, D18306,(2005)

© NMISA 2012


Effect of change in scales NOAA04 (solid) and CMDL83 (dashed)

E.J. Dlugokencky et al., J. Geophys. Res., 110, D18306,(2005)

© NMISA 2012

CCQM-P41, Methane 1.8 µmol/mol (2003)


DQO= ± 2.0 nmol/mol = ± 0.1%

© NMISA 2012

WMO Scale for Nitrous Oxide

NOAA-2006 N 2O replaces previous NOAA 2000 scale

NOAA-2006 scale defined by 13 primary standards pre pared gravimetrically (260-370) nmol/mol

Y= -2.2025·10-7 x3 + 1.20704·10-4 x2 + 0.98343 x

Difference between Scales

© NMISA 2012

CCQM-K68 (Nitrous oxide)

Coordinator KRISS

NMIJ NIM VSL NIST IMK-IFU GMD VNIIM KRISS

DQO= ± 0.1 nmol/mol

© NMISA 2012

BIPM-NIST programme to maintain the comparability of the worldwide network of ozone

reference standards

Surface Ozone Monitoring

© NMISA 2012

The reference method: UV photometry

BIPM – SRP27

OZONE SAMPLE

LIGHT

INTENSITY I0

ATTENUATED LIGHT

INTENSITY I

Light Path length 2l

σσσσ Ozone absorption cross-section at 253.64 nm under standard conditions of

temperature and pressure

T Temperature in the cells

P Pressure in the cells

R Gas constant

NA Avogadro constant

D Product of transmittance of the two cells

Lopt light path length

1ln( )

2 opt A

T Rx D

L P Nσ−=

x mole fraction of ozone in dry air (nmol/mol)

© NMISA 2012

Pilot study CCQM-P28 Final results - Di at 420

nmol/mol

NIS

T

ISC

III

ER

LAP

Env

ironm

ent C

anad

a

ME

TAS

SR

P18

ME

TAS

SR

P14

KR

ISS

LNE

VN

IIM FMI

WM

O/W

CC

-EM

PA

UB

A (A

)

SP

NP

L

ND

EN

W

UB

A (D

)

NIE

S

CH

MI

CS

IR-N

ML(

1)

NE

RI

NIL

U

NM

i-VS

L

INR

IM

CS

IR-N

ML

(2)

BIP

M G

PT

NIE

S G

PT-20

-15

-10

-5

0

5

10

15

20

Di (

nmol

/mol

)

(k=2)

i LABi BIPMD x x= −

© NMISA 2012

Classifying GAWG key comparisons

• “Analytical challenge”

• Species (and concentrations) for which

• analysis is challenging,• may not be stable in

cylinders• preparation of standards

may be complex

“Core”

Species (and concentrations) for which

• analysis based on “generic” techniques

• stable in cylinders• standards prepared from

gases

“Natural gas”

Species (and concentrations)• C3 and below (+ CO2 and N2) �� “core”• C4 and above (+ He) �� “analytical challenge”

© NMISA 2012

1.00E-01 1.00E-02 1.00E-03 1.00E-04 1.00E-05 1.00E-06 1.00E-07 1.00E-08 1.00E-09 1.00E-10 Mass FractionAnalyteCO2COC3H8CH4

19931994

SO2 1995NO 1996Ozone 1997NO2 1998

19992000

BTX 2001VOCs 2002SF6 2003CFCs 2004

2005EtOH 2006

Nat. Gas

H2SH2S/methaneNH3HCHOHClO2/N2H2ON2OPurityCS2

Mass Fraction10% 1 ppb

“Core species” and key comparisons

© NMISA 2012

Chemistry BIPM Impact: Improvements in Laboratory

Performance

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

2001 2002 2003 2004 2005 2006 2007 2008 2009

Year

Ave

rage

Rel

ativ

e S

tand

ard

Dev

iatio

n (%

)

All results

NMIs and DIs

u(xi) SRP

EUROMET 414

CCQM-P28

BIPM.QM-K1 Cycle 1

© NMISA 2012

243 244 2459.0

9.2

9.4

9.6

9.8

Burrows (1997) Malicet (1993) Bogumil (2004) This work, referenced to Hearn This work, referenced to BDM

Abs

orpt

ion

cros

s se

ctio

n /

(10-1

8 cm

2 /mol

ecul

e)

Wavelength / nm

Paper in press with Journal of Geophysical

Research – Atmospheres

244.1 nm

Ozone absorption Cross Section Determinations at th e BIPM

Relative measurements of ozone absorption cross-

sections at three wavelengths in the Hartley band using a well-defined

UV laser beam (2012)

Current activities• Pure ozone generation and

characterization• Path length measurements• Absolute X-section measurements

© NMISA 2012

Pilot study CCQM-P28 Final results - Di at 420

nmol/mol

NIS

T

ISC

III

ER

LAP

Env

ironm

ent C

anad

a

ME

TAS

SR

P18

ME

TAS

SR

P14

KR

ISS

LNE

VN

IIM FMI

WM

O/W

CC

-EM

PA

UB

A (A

)

SP

NP

L

ND

EN

W

UB

A (D

)

NIE

S

CH

MI

CS

IR-N

ML(

1)

NE

RI

NIL

U

NM

i-VS

L

INR

IM

CS

IR-N

ML

(2)

BIP

M G

PT

NIE

S G

PT-20

-15

-10

-5

0

5

10

15

20

Di (

nmol

/mol

)

(k=2)

i LABi BIPMD x x= −

© NMISA 2012

VOC target compounds; WMO-GAW Strategic Plan

2008-2015

17 target compounds• ozone formation

• fugitive emissions• biogenic emissions

• biomass burning• aerosol precursors• ocean emissions

60

© NMISA 2012

The GAW-VOC Target Compounds

∗ formaldehyde is discussed elsewhere.

Ozone precursor compounds in Europe (EU Ozone Directive 2002/3/EC) available in a standard certified by NMIs.

© NMISA 2012

Primary standards from NPL: CCL for VOCs

• Primary standards prepared and maintained by NPL

• Comparison with other NMIs verifies their accuracy

• Extensive stability trials by NPL confirms drift of<0.1% per year.

© NMISA 2012

Future – other VOCs

• “other VOCs (semi-stable)”

Permeation

� Need a dynamic dilution device to dilute standards from high-pressure

gas cylinders by a factor of 500 in air

© NMISA 2012GAS2011 symposium, Rotterdam, Netherlands, 9-11 February 2011

WMO/GAW Network : monitoring HCHO in the

background air

Global Atmospheric Watch (GAW)

© NMISA 201225th GAWG meeting, Sèvres, France, 11-12 April 2011

CCQM-K90: Formaldehyde Facility and

Comparison

2010

Permeation rate

analysis (temperature,

flows, …)

FTIR analysis - Impurities from permeation system?

Impurities from cylinders?

0.81000 1500 2000 2500 3000 3500 4000

0.0

0.2

0.4

0.6

0.8

-1

measured spectra, xHCHO

= 13 µmol.mol-1

Abs

orba

nce

DecJan …. DecJanDec…..AprJan

2011 2012

Cylinders validation studies

Jan

2013

International comparison

2009

DecJan Apr

Setup and validation

of the facility

…..….. Aug ….. ….. …..

Transfer standards issues

- concentration (1-10 ppm)

- stability

- purity

- provider !!!

© NMISA 2012

• Report of GAW Workshop on NOxy

• now published (WMO Report #195)

69

WMO / BIPM Workshopactions and recommendations

© NMISA 2012

70

Air Quality Gas Standard Comparison Facilities: NO 2

-1.500

-1.350

-1.200

-1.050

-0.900

-0.750

-0.600

-0.450

-0.300

-0.150

0.000

0.150

0.300

0.450

0.600

0.750

0.900

1.050

1.200

1.350

1.500

1.650

Laboratory

D (µ

mol

/mol

)

NPL NIM SMU NMIA NMISA CERI METAS I.N.RI.M KRISS FMI LNE NIST VSL CEM VNIIM BAM BIPM

WMO-GAW NOxy Monitoring

BIPM Primary Dynamic NO 2

Standard Facility

CCQM-K74 Coordinated by the BIPM:

17 Participating Laboratories

Key Comparison Reference Value based on BIPM Measurement Capabilities

© NMISA 2012

Conclusions

� 10 years of increasing collaborative work between W MO andBIPM-CCQM-GAWG Laboratories

� DQOs of WMO -GAW are more stringent than currentlyachievable uncertainties on primary gas standards

� WMO has adopted traceability to specific sets of st andards(scales) – requiring ultra stable gas standards

� NMIs can help established WMO -CCLs monitor changes andconsistenecy in their standards: Requires additional effort from NMIs

� Further requests from WMO for NMIs to act as CCLs expected

© NMISA 2012

Role and Mandate of the NMISA

The NMISA is mandated to keep, maintain and disseminate the National Measurement Standards and demonstrate

measurement equivalence for SA and the region (Act No. 18 of 2006)

In addition the NMISA is responsible for the application and maintenance of the Units (SI) in SA

The NMISA also performs reference analysis and in a dispute, in any SA court, its results will be accepted as

the most correct value

© NMISA 2012

NMISA Products and Services

National Measurement

Standards

Gazetted NMS

Gazetted NMS Primary Primary SecondarySecondary TransferTransfer

Reference Methods

Disseminate NMS

Disseminate NMS

Internationally benchmarkedInternationally benchmarked ValidatedValidated

Certified Reference Materials

Certified Reference Materials

Reference standards

Accredited Laboratory Traceability

Accredited Laboratory Traceability

Legal & Trade

Metrology

Legal & Trade

MetrologyIndustryIndustry

Consultation/R&D projects

Industry measurement

solutions

Industry measurement

solutions

Measurements for product

development

Measurements for product

development

NMS development & Improvement

NMS development & Improvement

Knowledge dissemination/Collaboration

PublicationsPublications Conference presentationsConference

presentationsTraining coursesTraining courses

Exchange/ assistance programs

Exchange/ assistance programs

Comparisons/Reference measurements

CIPMCIPM RegionalRegional Bi-lateral

Bi-lateral

SANAS PT scheme

SANAS PT scheme

© NMISA 2012

NMISA Activities: Chemistry

Chemical Traceability

Reference Measurements

Instrument calibration

Ozone metersBreathalysers

Samples/ PT

EnvironmentalFood safety

EnergyAutomotive emissions

REACH/RoHSNano/biotechnology

Pharmaceutical

Reference Materials

Pure mixtures (calibration)

Elemental solutionsGas PRMs

EtOH & NaF CRMs

Matrix (bias)Various in Food and

Environmental matrices

© NMISA 2012NMISA 2011

Nutritional content

Protein content: amino acid

SAGL PT scheme

Mycotoxins

Multiple toxins in maize &

wine

SAGL PT scheme

Wine industry

Pesticide residues

Fruits & vegetables

PT schemes/ referencemeasure-ment ISO

17025 labs

Veterinary drug residues

Chloram-phenicolin pork

and milk

Veterinary Institutes

& Meat industry

Processing contaminants

Melamine in infant

formula & milk,

methoxy-pyrazines

in wine

Dairy & wine

industry

Industrial & environ-mental

chemicals

POPs

Chemistry for Food Safety Regulations

© NMISA 2012

Gas Metrology

• GC-FID/ PDHID, FTIR, NDIR, GC-MSD and CRDS

• Preparation of primary gas reference mixtures by gravimetry in N2 and air matrices

• CO2 ;CO;NO;NO2;SO2;H2S;C3H8;Stack gas mixtures

• Purity analysis • Calibration of breathalysers• Calibration of air pollution analysers• Certification of gas mixtures• Uncertainty in Chemical Measurement

© NMISA 2012

Inorganic Chemistry

• What’s in it?• ICP-MS, LA-ICP-MS, ICP-OES• Trace and ultra-trace element analysis in food

and environmental samples• Se in wheat • Sn in tomato paste• Cd in rice• Pd, Cd, Ca, Fe in wine• Ca, Fe, Cu, Zn in fat soybean• Cd, Fe, Pb and Zn in bovine liver• Cd, Cr, Ni, Hg, Pb and Pt in algae

• Metals in manufacturing materials• Cr, Mn, Mo and Ni in low alloy steel• RoHS (Cd, Cr, Hg and Pb) in polypropylene• Pb in lead-free solder

• Application: Reference analysis and certification of materials/ foods

© NMISA 2012

• Temperature & Humidity • Extended temperature scale• New humidity standards

• Photometry & Radiometry• Light and colour• Energy efficient lighting (LEDs)• Expand solar irradiance measurement to

include solar UV measurement• Support to satellites such as SumbandilaSAT• New spectral irradiance lamps for the UV

region, new UVA/B/C sources and detectors

NMISA Activities: Electricity and Magnetism

© NMISA 2012

NMISA Activities: Ionising Radiation

Dosimetry Radioactivity

Parameters-Dosimetry: *Absorbed dose to water*Air kerma*Ambient dosimetry*Personal dosimetry-Radioactivity:

* Surface emission rate

Methods for activity measurements

-TDCR efficiency-CIEMAT/NIST method-4πβ-γ and 4π(x,e)-γ coincidence * Double NaI(Tl) detector for γ-rays* Ionization chamber

Assisting the National Nuclear Regulatorwith establishment of Reference Laboratory

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