Metrohm White Paper

Boost efficiency in the QC laboratory:

How NIRS helps reduce costs up to 90%

Nicolas Rühl, Ph.D. and

Alyson Lanciki, Ph.D.
Underestimation of quality control (QC)
processes is one of the major factors leading
to internal and external product failure,
which have been reported to cause a loss
of turnover between 10–30%. As a result,
many different norms are put in place
to support manufacturers with their QC
process. However, time to result and the
associated costs for chemicals can be quite
excessive, leading many companies to
implement near-infrared spectroscopy (NIRS)
in their QC process. This paper illustrates
the potential of NIRS and displays cost
saving potentials up to 90%.

Metrohm International Headquarters; Herisau, Switzerland

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 Metrohm White Paper
Quality Control with NIR Spectroscopy –
A sustainable boost in efficiency
«Good quality is expensive.» One could argue that high One strategy could be to analyze each of these action points
product prices are often due to costly production processes, individually, in order to find any major gaps as well as to define
which result from extensive quality control (QC) and quality the respective countermeasures. Alternatively, companies can
assurance (QA) measures. However, as a QA/QC Manager, also take advantage of more modern QC technologies which
you might disagree and refer to personal examples and have the potential to address all four of these approaches
scientific studies outlining the consequences of poor quality directly.
control measures. The following white paper provides a
short summary about the importance of QC and QA, while Near-Infrared Spectroscopy (NIRS) is an example of a modern
illustrating action points to improve existing QC processes. QC method which significantly boosts the efficiency of QC
Furthermore, near-infrared (NIR) spectroscopy is presented as labs. In the following section, this technology and its benefits
a powerful analysis technique to increase QC efficiency while are presented and discussed.
maintaining the accuracy and precision of the existing analysis
method. Near-Infrared Spectroscopy (NIRS)
All spectroscopic methods determine sample properties by
The importance of QC and QA analyzing the specific interaction between light and matter.
Two main failure costs are addressed and mitigated with a This interaction varies in dependence of the applied light
reasonable QC/QA framework in place: source, and therefore the different spectroscopic technologies
are defined by the applied light energy (i.e. wavelength), and
• Avoidance of internal failure by the type of interaction. With NIRS, for example, instruments
• Avoidance of external failure detect the quantity of absorbed (absorbance spectroscopy)
near-infrared light (NIR = 800–2500 nm respectively
Internal failure costs are associated with internal errors (e.g. re-
12500–4000 cm-1, see Figure 1) by functional groups such as
inspection, rework, or scrapping). External failures are related
-CH, -NH, -SH, or -OH.
to product defects found after delivery to the customer. These
are expensive and involve a significant risk because they
can affect brand reputation or even induce a loss of market O H
share. Follow-up actions such as warranties, repairs, or recalls, N
N
require a great expenditure and therefore will significantly O H n n
reduce revenues.
Nylon Polyethylene
To avoid these failures and their related costs, it is advisable
to invest reasonably into prevention measures. One such
activity is the continuous monitoring of used raw materials,
intermediate products, and final products. More commonly,
companies prefer to gamble by under-investing in this area
and neglect the negative implications, which can result in a
loss of turnover between 10–30%.[1]

Aside from implementing the appropriate checks along

the complete production process, companies should also
challenge their existing QC processes and setups in order
to discover how to further increase production efficiency.
Possible approaches include:

• Reduce budget for testing and inspection

• Increase efficiency of production equipment
• Improve productivity of the operators
• Make manufacturing easier Figure 1. Comparison of spectra taken from Nylon and polyethylene
in the near-infrared wavelength region. The differences seen are due
to their different chemical structures – Nylon contains nitrogen func-
tional groups whereas polyethylene does not.

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Since the NIR light-matter interaction is by nature fast and non- In regards to the action points to improve QC efficiency on
destructive, NIRS-based analytical methods offer significant the previous page, it is apparent that companies which have
advantages over conventional approaches. Samples are implemented NIRS methods into their routine QC testing
analyzed as-is without time-consuming preparative steps, and are able to reduce their testing budget and improve their
remain undamaged. All NIR-sensitive information is gathered operators’ efficiency at the same time. Table 1 and Figure 2
by a single measurement in less than one minute, and is present the potential return on investment (ROI) by comparing
displayed in the spectroscopy software as a spectrum. analysis costs per year between the commonly used methods
of titration and viscometry versus near-infrared spectroscopy.
The action of acquiring a quick and complete overview of
information is identical to the experience of capturing the
image of an object with a camera. A single picture includes
all sorts of information about the object e.g. color, size, Running Costs / Year
shape, position, etc. Analogous to the picture, a spectrum $500,000
is a complete scan which includes numerous information
$400,000
about the sample (e.g. the water content, OH-Number,
viscosity, or the acid number). For both the camera image $300,000
and sample spectra, the only necessary action is to interpret $200,000
the data, which in the case of NIRS is performed by the
provided manufacturer spectroscopy software. $100,000

$0
1 2 3 4 5 6 7 8 9 10
Currently, manufacturers of NIR instruments pay particular Cumulative costs: Primary Cumulative costs: NIR Savings
attention to the convenience of system operation, resulting
in standardized analyzers and easily defined operating Figure 2. Possible return on investment as related to running costs
procedures. Both facets simplify the implementation of NIR when analyses are conducted with NIRS vs primary methods.
spectroscopy into daily QC operations, even across multiple
locations, requiring only minimal training of the operators.

Table 1. Overview of estimated costs for the analysis of different parameters with primary methods vs NIRS. The full ROI is achieved within
11 months.

Total analyses per day 10 10

Cost of operator per hour $ 25 $ 25
Cost of Analyzer Primary Method Near-Infrared Spectroscopy
DS2500 Analyzer — $ 55,000
1
Total initial costs $0 $ 55,000
Running costs consumables and/or chemicals: per analysis
Determination of H2O content (ISO 15512) $5 $0
Determination of functional groups $5 $0
Determination of viscosity (ISO 307) $6 $0
Total costs consumables and/or chemicals: per year $ 35,100 $ 0.00
Time spent per analysis (minutes)
Determination of H2O content (ISO 15512) 5.0 0.5
Determination of functional groups 5.0 0.5
Determination of viscosity (ISO 307) 15.0 0.5
Total yearly labor costs $ 23,438 $ 469
Total running costs $ 58,538 $ 469
1
Assumption that the instrument had previously been purchased, and therefore this cost is not included in the ROI calculation.

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Application Examples

Some key parameters have already been mentioned in the In the following section, three different industries and
previous chapter, however a complete list of possible NIRS application examples are described. However, it is important
applications would exceed the scope of this paper. Typical to note that the precision values are a function of the chosen
industries where NIRS is an established analytical QC method concentration range. Therefore, selecting lower concentration
include: ranges will most likely further enhance the precision of the
results.
• chemicals
• lubricants
• petrochemicals
• polymers
• paint, inks, and dyes
• pulp and paper
• pharmaceuticals
• personal care and cosmetics
• food and feed, agriculture

Chemical Industry – Polyols

Polyols, a class of organic compounds characterized by the Table 2. Overview of typical parameters measured in the polyol
presence of two or more hydroxyl groups, are crucial starting industry which can also be analyzed by NIR spectroscopy.
materials for the production of polyurethanes. Both the
reaction behavior of polyols and the composition of the final Parameter (unit) Range Precision
product are highly dependent on the number of hydroxyl Hydroxyl Value (mg KOH/g) 70.00–125.00 0.68
groups, which makes the analysis of this functional group so
Acid Value (mg KOH/g) 0.10–8.00 0.38
important. The reactivity of polyols also depends upon their
moisture content and the acidity represented by the number Moisture content (mg/L) 75–400 52
of attached carboxylic acid groups.

NIRS is an established technology for the analysis of polyols

(ASTM D6342), able to precisely determine all three
parameters within 30 seconds as shown in several applications 220
Hydroxyl Number NIR value: mg KOH/g

[2]. Table 2 presents some key results from a polyol analysis

200
utilizing NIR spectroscopy.
180

160

140
Absorbance

120

100

80
400 700 1100 1300 1600 1900 2200 2500 80 100 120 140 160 180 200 220
Wavelength / nm Hydroxyl Number lab value: mg KOH/g

Figure 3. NIR spectra taken of polyol samples with varying OH num- Figure 4. Correlation plot comparing NIRS to a primary laboratory
ber values. method.

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Polymer Industry – 2.5

Polyethylene terephthalate

DEG NIR value: %

2.1

Polyethylene terephthalate (PET) is one of the most produced

polymers worldwide, next to polyethylene and polypropylene. 1.7
Raw materials for the production of PET include diethylene
glycol along with either dimethyl terephthalate or terephthalic
1.3
acid during transesterification and esterification reactions.
1.3 1.7 2.1 2.5

Product quality is primarily determined by the content of DEG titration value: %

diethylene glycol (DEG) and isophthalic acid (which reduces
4.5
the crystallinity of PET). Additionally, the intrinsic viscosity (IV)
(ASTM D4603) and the acid number (AN) are important

IPA NIR value: %

parameters to control in order to avoid external failures. NIRS
has proven its validity as an analytical method which reliably
3.0
determines these parameters. Table 3 displays the respective
concentration ranges and precision values for this application
as described in the Metrohm Application Note NIR-023 [3].

1.5
1.5 3.0 4.5
Table 3. Overview of typical parameters measured in the polymer IPA titration value: %
industry which can also be analyzed by NIR spectroscopy.
6.0

Parameter (unit) Range Precision 5.0

AN NIR value

Diethylene glycol content (%) 1.4–2.0 0.066 4.0

Isophthalic acid content (%) 1.8–4.5 0.143
3.0
Intrinsic viscosity 0.5–0.9 0.024
2.0
Acid number 1.2–6.0 0.143
1.0
1.0 2.0 3.0 4.0 5.0 6.0
AN titration value

Figure 5. Correlation plots for NIRS compared to laboratory primary

methods for diethylene glycol (DEG), isophthalic acid (IPA), and acid
number (AN).

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Petrochemical Market –
Gasoline
Gasoline is one of several end products resulting from a
complex production chain starting with the refinement of
crude oil. This fuel product requires intensive checks on several
quality parameters which need to be within specification
before commercialization. These parameters, which can also
be controlled by NIR analysis include the Research Octane
Number (RON) and Motor Octane Number (MON), the olefins,
oxygen, aromatic content, and the density.

The importance of measuring these values precisely is not

just related to regulations, but this also offers manufacturers
further potential to save costs. As an example, RON values Table 4. Overview of typical parameters measured in the
exceeding the requirement will still be accepted by the market, petrochemical industry which can also be analyzed by NIR
but these products include a higher amount of lucrative long- spectroscopy.
chain organic molecules. This so-called «RON give away»
(Figure 6) is estimated at approximately 0.5 RON per Parameter (unit) Range Precision
barrel, resulting in 2.25 million USD/month in lost revenue RON 85.00–94.00 0.68
for a production of 100,000 barrels per day. MON 81.00–100.00 0.53

Ready-to-use NIRS systems are available for monitoring Olefins (%) 1.0–25.0 1.3
several gasoline parameters, which cover varied ranges and Oxygen (%) 0.200–2.000 0.045
their respective precisions, shown in Table 4. Additionally, Aromatics (%) 20.0–45.0 1.1
the manufacturers of NIRS analyzers usually offer application 3
support to extend these ranges or improve upon the precision. Density (g/cm ) 0.7400–0.7600 0.0024

ASTM Reproducibility

Supplier Testing Margin

Refinery Site Precision

ASTM Repeatability

ASTM Report interval

EN228 Specification Give Away range

Recipient Testing Margin

94.0 94.2 94.4 94.6 94.8 95.0 95.2 95.4 95.6 95.8
RON
Figure 6. Overview of typical RON give aways in relation to different methods.

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Summary

At first glance, investment into quality control might increase

product costs. However, this reduces costs related to external
and internal failures, which are of higher magnitude and have
the potential to reduce up to 30% of the turnover.

Besides enforcing a reasonable quality control program,

the efficiency of the QC and QA department is required to
produce materials cost-effectively. One way to achieve this is
to implement modern, easy to use, fast QC methods. NIRS is
an established methodology used across different industries.
This technique combines these requirements and provides
significant potential to reduce costs and increase operator
efficiency.

References

[1] Why Improving Quality Leads to Lower Manufacturing Costs, QualityInspection.org. (accessed October 30, 2019).
https://qualityinspection.org/improving-quality-cost-china/

[2] Metrohm Application Note NIR-035 Hydoxyl number in liquid polyols using Vis-NIR spectroscopy
https://www.metrohm.com/en/applications/AN-NIR-035

[3] Metrohm Application Note NIR-023 Diethylene glycol, isophthalic acid, intrinsic viscosity, and acid number in PET
granulate by NIRS
https://www.metrohm.com/en/applications/AN-NIR-023
WP-054EN by Metrohm, published 02-2020

Contact: info@metrohm.com